Recent News and Scientific Developments!

Triclinic Labs, Inc., a Food and Drug Administration (FDA) registered contract pharmaceutical physical, organic, and analytical chemistry laboratory which follows Good Manufacturing Practices (cGMP) completed an unannounced inspection by the agency over two days from January 16 through January 17th, 2024. This was a GMP surveillance establishment inspection of our facilities conducted in accordance with compliance program CP 7356.002 Drug Manufacturing Inspections. There were no FDA findings and the inspection was classified as “No Action Indicated “, or NAI. No refusals were encountered, and no samples were collected. Ms. Brandi Albea, Triclinic Labs’ Director of Quality Systems led the inspection. “We are pleased the FDA was able to complete their inspection of our facilities, SOPs, and systems and depart with no findings and no 483s” she said. “It speaks to the tremendous effort and investment Triclinic has made in subject matter experts and systems to support our clients in their cGMP testing and release efforts” she added.

Triclinic Labs offers leading analytical testing, method development, validation, and release testing of pharmaceuticals, medical devices, and other specialty chemicals. They are specialists in solid-state materials characterization.

For more information on how Triclinic Labs can assist with cGMP analysis please request a free consultation by clicking here. To contact Brandi Albea directly, you may email her at rfi@tricliniclabs.com.

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Triclinic Labs, Inc. is pleased to announce it now offers Amorphous Solid Dispersion Developement for preclinical use. Amorphous solid dispersions are a proven approach to alter the properties of active pharmaceutical ingredients (API) for improved dissolution rate, solubility and overall bioavailability, and produce added intellectual property. Triclinic offers amorphous solid dispersion (ASD) development as part of our solid form screening and development services. Polymers are utilized in spray drying and hot-melt extrusion to improve the solid-state stability of amorphous solid dispersions. Feasibility studies allow us to quickly and cost effectively determine if the formulation will lead to improved properties. The lab scale process can be scaled up to meet clinical and production needs. We have numerous case studies that demonstrate these techniques are viable approaches for molecules with both solubility and stability issues.

At Triclinic, the following considerations are evaluated in ASD development:

• API: Is the API a fast or slow crystallizer? What is the solubility advantage of the amorphous form?
• ASD: Which polymer from a toolbox of 8-12 proven additives, is best? What is the best drug loading (%w/w)?
• Processing: Should the ASD be generated via solvent- or melt-based approach?
• Stability: What are the recommended storage conditions? How does temperature and humidity affect stability?
• Performance: Does the ASD show superior performance during in vitro dissolution compared to its crystalline counterpart?

Triclinic Labs is equipped with a ProCept R&D spray dryer and a MiniCTW hot melt extruder. The entire ASD development can be performed with as low as 500 mg material. In addition, Triclinic Labs is equipped with complete thermal, microscopy, and spectroscopy techniques sensitive for crystallization detection needed in an ASD development. For more information including case studies, please click here.

For more information on how Triclinic Labs can assist with ASD Development, please request a free consultation by clicking here. To contact Dr. Nico Setiawan directly, you may email him at NSetiawan@TriclinicLabs.com.

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Triclinic Labs, Inc. is pleased to announce it has completed cGMP Qualification of its 400MHz Bruker NEO Nuclear Magnetic Resonance (NMR) spectrometer. Due to overwhelming client requests for cGMP NMR services, Triclinic invested heavily in upgrades and in making the instrument compliant with federal regulations for the pharmaceutical industry, including validating the instrument software.

Dr. Byungsu Kwon who leads Triclinic Labs' solids and liquids NMR Analysis group announced the new capabilities: "NMR has become a vital technique for chemical development companies not only for structure elucidation but also for use in Chemistry Manufacturing and Control (CMC) requirements. In support of The United States Pharmacopoeia (USP) General Chapter <761> Nuclear Magnetic Resonance Spectroscopy and other Compendial chapters (e.g., <1761>), Triclinic Labs offers multi-dimensional cGMP liquids analysis with a broadband probe allowing for a myriad of experiments (1H, 13C, 15N, 19F, 31P, etc.) at variable temperatures (280K (7C) to 323K (50C)). Our solid-state services, although currently non-GMP, are provided via a 4 mm Cross-Polarization Magic Angle Spinning (CPMAS) probe and associated high-power amplifiers for broadband solid-state NMR analysis.

In addition to the requirements described in the USP documents, any analytical system used for the creation of analysis data for pharmaceuticals must also comply with the US Food and Drug Administration’s (FDA) 21 CFR Part 11 regulations regarding electronic records and validation of electronic signatures. Triclinic Labs has qualified the instrument for cGMP use and has validated the software for compliance. Dr. Kwon stated "Our cGMP NMR analysis capabilities also include method development, validation, and release testing."

For more information on how Triclinic Labs can assist with cGMP NMR sample analysis needs, please request a free consultation by clicking here. To contact Dr. Byungsu Kwon, you may email him at BKwon@TriclinicLabs.com.

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Today, Triclinic Labs announced it had completed installation and performance testing using model systems, of the new Anton Paar CHCplus Cryo and Humidity Chamber with Liquid Nitrogen Cooling. This system offers a unique combination of temperature and humidity control for real-time observation of structural changes in materials under non-ambient conditions using powder X-ray diffraction.
Steef Boerrigter, Ph.D. who leads the materials modeling group at Triclinic Labs stated: “This instrumentation combination enables in situ characterization under an incredibly wide range of working conditions you might encounter in development, manufacturing, and storage. When combined with differential scanning calorimetry, thermo-gravitational analysis, and/or dynamic vapor sorption analysis, it offers an incredibly deep understanding of phase transitions that is otherwise very difficult or impossible to attain. In addition to equilibration studies, scanning mode analysis offers a view of the rate and dynamics of the phase transitions.”
Often referred to as Variable Temperature - Variable Relative Humidity Powder X-ray Diffraction (VT/VRH-PXRD). This new addition supports investigations into pharmaceuticals, fine chemicals, and clays or zeolites in humid air, inert gazes, or vacuum. Due to its versatility, the new VT/VRH-PXRD setup opens new dimensions in analysis for materials science.
The VT/VRH-PXRD system at Triclinic Labs offers the following features:

• 2% to 95% relative humidity with variable temperature from 10 to 80 C,
• -5°C to +300°C in air or dry nitrogen,
• -120 C to +300 C using liquid nitrogen cooling system,
• -180 C to +400 C using liquid nitrogen cooling system and vacuum,
• Atmospheres: vacuum (< 10-2 mbar), air, inert gasses,
• Reflection-geometry PXRD in 2θ range of 0°-164°,
• Data collection strategies include program-controlled VT/VRH points or continuous scanning modes.

For more information on how Triclinic Labs can assist with in-situ VT/VRH-PXRD sample analysis needs, please request a free consultation by clicking here. To contact Steef Boerrigter, you may email him at SBoeriggter@TriclinicLabs.com.

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Triclinic Labs, Inc. announced it has added to its elemental analysis capabilities with the addition of a latest generation Thermo Scientific iCAP RQ Inductively Coupled Plasma - Mass Spectrometer (ICP-MS).

Dr. Jeff Stewart who leads Triclinic Labs' chromatography and elemental analysis group announced the new capabilities: "Impurities in pharmaceutical products are of great concern not only due to the inherent toxicity of certain contaminants, but also due to the adverse effects that contaminants may have on drug stability and shelf-life. This necessitates the monitoring of organic and inorganic impurities throughout the pharmaceutical manufacturing process, from raw ingredients to final products. This innovative single quadrupole (SQ) ICP-MS is the ideal trace elemental analyzer for a wide range of sample types."

The United States Pharmacopoeia (USP) General Chapter <232> Elemental Impurities - Limits, defines the maximum limits of fifteen elements in pharmaceutical products and Chapter <233> Elemental Impurities - Procedures, defines how the testing for these elements should be performed.

“We have successfully demonstrated that the new ICP-MS can accurately and reproducibly quantify the fifteen (15) target elements in USP<232> with exceptionally low detection limits and across a wide variety of drug products and substances in accordance with USP<233>,” Dr. Stewart continued.

In addition to the requirements described in the USP documents, any analytical system used for the creation of analysis data for pharmaceuticals must also comply with the US Food and Drug Administration's (FDA) 21 CFR Part 11 regulations regarding electronic records and validation of electronic signatures. Triclinic Labs is currently qualifying the instrument for cGMP use and validating the software for compliance. Dr. Stewart stated "We should have cGMP analysis capabilities including method development and validation ready in a few months, but in the meantime we can quickly accommodate elemental testing across a wide variety of industries."

For more information on how Triclinic Labs can assist with your elemental sample analysis needs, please request a free consultation by clicking here. To contact Jeff Stewart, you may email him at JStewart@TriclinicLabs.com.

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Triclinic Labs, Inc. was featured in the January/February 2023 edition of Drug Development & Delivery Magazine. The Special Feature - Outsourcing Analytical Testing - Timelines, Regulations & Biologics Drive the Sector in the Analytical Testing, Contract Services, Featured Articles, Formulation Development section highlights new developments in the lab. In this exclusive Drug Development & Delivery annual report, leading contract development and manufacturing organizations (CDMOs) discuss not just their analytical service offerings, but their strategies for meeting regulatory challenges and ensuring faster project timelines.

To read the entire article please click here.

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Triclinic Labs, Inc. announced that it has installed a new Renishaw RA802 Pharmaceutical Analyzer. The system is designed for Raman spectral analysis and rapid imaging using near infrared excitation at 785 nm. The new system features a HSES motorized XYZ microscope stage to allow scatter, line, and area mapping, and confocal depth profiling and the StreamLine fast imaging technology enables users to produce Raman chemical images rapidly.

“This new system complements our existing Renishaw Dispersive Microscope by allowing nearly automated, rapid, drug product imaging but at a much faster rate” said David Bugay, Ph.D., Triclinic’s CSO. “Clients have requested drug product and other volume reconstruction services and this system gives us the imaging speed to do that cost effectively when paired with our microtomy systems” he continued. The new system also allows quantification of image domains and particle characteristics including area, equivalent circle diameter, perimeter, eccentricity, orientation, solidity, and nearest-neighbor distance.

For more information on how Triclinic Labs can help you in drug product analysis, failure identification, and intellectual property development, please request a free consultation by clicking here. To contact David Bugay, you may email him at DBugay@TriclinicLabs.com or phone at +1.765.588-5631.

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Triclinic Labs, Inc. announced that it has completed the Phase II expansion of its laboratory space.

The approximately 5000 square feet of new laboratory space includes dedicated areas for physical chemistry, chemical synthesis, materials characterization, and formulation development. In addition to six hoods, one walk in hood, and an environmentally controlled space for Mass Spectrometry, Triclinic invested more than two million dollars in new equipment and capabilities.

"We are excited to open the new space which will not only provide significantly more capacity for solid form screening projects, but also delivers the needed space for new services like ICP-MS, spray drying, and amorphous formulation development." said Dr. Aeri Park, Triclinic's Chief Operating Officer. "We have added space as well as subject matter experts over the last six months to meet client demands and it's great to finally put both capabilities together," she continued.

For more information on how Triclinic Labs can help you in pre formulation and formulation development , please request a free consultation by clicking here. To contact Aeri Park, you may email her at APark@TriclinicLabs.com or phone at +1.765.588-9538.

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Triclinic Labs, Inc. announced Nico Setiawan, Ph.D. has recently accepted a position as Senior Research Scientist in the physical and analytical chemistry groups. He will focus his efforts on active research and development projects and the addition of new preformulation and formulation capabilities.

Dr. Nico Setiawan received his Ph.D. in Pharmaceutical Science from the University of Kentucky. Nico is an expert in the preformulation space of API development, including solid form screen and selection, solid-state and physicochemical characterization, crystallization process development, development of enabling formulation for poorly soluble compounds, and biorelevant dissolution method development for orally administered compounds. His research focuses on integrating properties of API and physiological barriers to deliver efficacious drug products. Dr. Setiawan has published papers in peer-reviewed journals and presented at national conferences. He is also an active reviewer of several peer-reviewed journals.

"We are incredibly pleased to have someone with Nico's formulation and solid-state screening experience join our company" said Dr. Aeri Park, Triclinic's Chief Scientific Officer. "We devote a considerable amount of resources for novel research and development projects and Nico will lead those efforts in addition to establishing preformulation and non-crystalline formulation capabilities that our clients have asked for," she continued.

For more information on how Triclinic Labs can help you in pre formulation and formulation , please request a free consultation by clicking here. To contact Nico Setiawan, you may email him at NSetiawan@TriclinicLabs.com or phone at +1.765.422.5009.

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Triclinic Labs, Inc. announced it has added to its X-ray analysis capabilities with user privledges at Argonne National Labs.

Dr. Steef Boerrigter who leads Triclinic's Materials Modeling group announced the new capabilities: "For highly accurate, high resolution XRPD data collection, synchrotron radiation can make a key difference. Triclinic is now an approved user at Argonne National Lab for collection of XRPD data. Our computational methods using synchrotron data push the boundaries far beyond the capabilities of in-house lab XRPD data for phase identification, structure elucidation, mixture analysis, and lowest level of detection for crystalline materials. Sample analysis typically takes a few weeks from receipt to final analysis."

The unique properties of synchrotron radiation are its continuous spectrum, high flux and brightness, and high coherence; which make it an indispensable tool in the exploration of materials. The wavelengths of the emitted photons span a range of dimensions from the atomic level to biological cells, thereby offering the possibility for advanced research in materials science, physical and chemical sciences, metrology, geosciences, environmental sciences, biosciences, medical sciences, and pharmaceutical sciences. The features of synchrotron radiation are especially well matched to the needs of nanoscience experiments.

“We have used synchrotron radiation and the subsequent high resolution data generated in legal matters for intellectual property support, crystal structure determination, and exploration of the structure of non-crystalline materials.” Dr. Boerrigter continued.

For more information on how Triclinic Labs can leverage synchrotron radiation and advanced data analysis for X-ray powder diffraction experiments, please request a free consultation by clicking here. To contact Steef Boerrigter, you may email him at SBoerrigter@TriclinicLabs.com or phone at +1.765.588.6200 ext 321.

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Triclinic Labs, Inc. welcomes Steef Boerrigter, Ph.D. as our new Research Fellow and Head of Materials Modeling.

Dr. Boerrigter received his Ph.D. in Computational Materials Science from Nijmegen University, The Netherlands, where his research focused on Crystal Morphology Prediction. Prior to joining Triclinic Labs, Dr. Boerrigter spent 12 years at AMRI (formerly SSCI, Inc.), where he advanced to the position of Senior Research Investigator. There he served as a group leader in materials science, focusing on polymorph, salt, and cocrystal screening, applying computational methods for solid-state characterization and phase transitions, as well as structure elucidation by single-crystal diffraction. At Triclinic, Dr. Boerrigter will lead the Materials Modeling group in both organic and inorganic analysis and expand method development and validation capabilities. He will lead complex analytical projects and will evaluate new instrumentation and techniques for inclusion in Triclinic’s service offerings. “This is truly an opportunity of a lifetime. My background is a perfect fit for this position and from day one, I felt right at home.” Dr. Boerrigter commented. “I am very excited to join this group of world-renowned experts in solid-state development.” he continued.

“We’re pleased to hire someone of Steef’s experience and knowledge” said Aeri Park Ph.D., Triclinic’s CSO. “He brings a wealth of ideas and approaches around structure elucidation, materials modeling, and prediction analysis - all of which greatly strengthens Triclinic’s capabilities in both routine as well as intellectual property investigations” she continued.

To contact Steef Boerrigter, you may email him at SBoerrigter@TriclinicLabs.com or phone at +1.765.588.6200 ext 321.

For more information on how Triclinic Labs can help strategically position your solid-state pharmaceutical programs for success using the most innovative development and analysis tools, please request a free consultation by clicking here.

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Today, Triclinic Labs announced it has completed Phase I of a two phase physical and capital expansion.
“We've experienced tremendous growth since our inception in 2009 and have already outgrown our fit-for-purpose laboratory facility that we opened in 2015” Shawn Comella, Triclinic's Chief Executive Officer said. “We've invested heavily in not only subject matter experts, but also instruments and infrastructure as we continue to build world-class cGMP and non GMP chemical development and materials characterization capabilities. We just finished the addition of phase I of a total of 4500 ft2 of new personal and laboratory space” he continued. In addition to a scientific office area, the new addition will house chromatography, mass spectrometry, and wet chemistry capabilities. This new area will allow Triclinic to add additional client requested capacity and capabilities.

To contact Triclinic for more info you may email us at RFI@TriclinicLabs.com or phone at +1.765.588.6200.

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Today, Triclinic Labs announced it has installed a nanoScience Instruments' Phenom XL G2 Scanning Electron Microscope (SEM) with Energy Dispersive X-ray elemental analysis capabilities.

We are excited to add the Phenom XL G2 SEM with EDS/X capabilities to the array of analytical instrumentation at Triclinic Labs. This instrument allows us to provide a multi-disciplinary approach to material characterization and contaminant analysis in conjunction with our current microscopy (optical and digital) and microspectroscopy capabilities (IR, Raman, and low frequency Raman)." said David Bugay, Ph.D., Triclinic's scientific principal.

"An exciting feature of the EDS/X detector is the ability to obtain elemental images of materials within the interior core of tablets and microspheres and interface this information with molecular information obtained from the other in-house microspectroscopy techniques. Using different data sources, Triclinic Labs is able to overlay SEM, EDS, IR, and Raman images with different levels of opacity, to fully characterize and view the properties and component distribution of solid-state pharmaceutical materials. The new system also includes Elemental Mapping application software for elemental identification and location and ParticleMetric software for analysis of particles. Finally, using a CeB6 source provides high brightness and a longer lifetime for the electron source resulting in superior quality images and less instrument downtime for source replacement Bugay commented.

For more information on Triclinic's new SEM/EDS capabilities or to contact Dave Bugay you may email him at DBugay@TriclinicLabs.com or phone at +1.765.588.5631.

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Today, Triclinic Labs announced it has promoted Dr. Aeri Park to the role of Chief Scientific Officer (CSO). Dr. Park received her Ph.D. from the University of Oklahoma and is a recognized industry expert in API solid form screening and selection, solid-state characterization of APIs, intermediates, and drug products, crystallization method development, patent prosecution support, and frequently acts as an expert witness in Paragraph IV litigation matters both domestically and internationally.

Dr. Park will lead Triclinic’s efforts in physical and analytical chemistry services as well as contribute to its patent prosecution and litigation expert services practice. Dr. Park joined Triclinic in 2017 as Vice President of Chemistry. Dr. Aeri Park, was formerly Director of US Operations for Almac Group and established and grew a US-based analytical laboratory for the firm. Prior to joining Almac, Dr. Park was instrumental in the growth and scientific success of SSCI, a solid-state development group.

“I’m excited to lead the Analytical Chemistry and Materials Characterization group” Dr. Park commented. “We've invested heavily in not only subject matter experts, but also instruments and infrastructure as we continue to build world-class cGMP and non GMP analytical capabilities. I'm excited to drive the next level of strategic growth.” she continued. “We are fortunate to have someone of Aeri's scientific capabilities and professional drive.” said Shawn Comella, Triclinic’s Chief Executive Officer. "She's done tremendous things in her short time at Triclinic and we look forward to seeing the new things she accomplishes." he added. Aeri replaces Dave Bugay, Ph.D. who is retiring and has transitioned to the role of Scientific Consultant.

To contact Aeri Park you may email her at APark@TriclinicLabs.com or phone at +1.765.588.9538.

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Simon Bates Ph.D. announced the publication of "Chapter 5.6. X-ray diffraction from non-crystalline materials: the Debye model in Volume H of the International Tables for Crystallography. In the chapter, the topic of X-ray diffraction from non-crystalline materials is introduced. A non-crystalline system can be considered to have a diffraction diagram that is essentially continuous with no discrete diffraction features. The Debye diffraction equation can be used to model the characteristic diffraction from residual local order based upon the coherent scattering between individual atom-atom pairs. The motivation behind this work as applied to organic molecular solid forms was the investigation of relationships between local molecular order and long-term chemical/physical stability, how changes in production conditions affect local order and long-term stability.

"I am excited to present this collaborative introductory chapter on amorphous diffraction analysis using DeBye diffraction theory Bates said. "While many people believe the 'amorphous halo' seen in non-crystalline materials' X-ray diffraction data is devoid of information, our research shows that not to be the case - much the opposite he continued. "This work not only illustrates alternative methods of analysis; it shows the data contained in that analysis can be used to solve crucial questions in drug development such as 'is my amorphous formulation stable?' Bates said. For more information on the aforementioned chapter please contact our materials modeling group at SBoerrigter@TriclinicLabs.com

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Today Triclinic Labs, Inc. celebrates its 10th anniversary as a contract physical and analytical chemistry development firm. Over the last ten years we've grown from (literally) three scared guys in a small lab with a few instruments to nearly 30 employees in a custom built 12,000 ft2 research and development space with nearly $10 million in capital. We're proud of our >98% customer repeat rate and nearly 100% employee retention level. Survival is rewarding - but seemingly scarce in drug development.

We don't want to be the biggest physical and analytical chemistry development group. Our single biggest goal is to continue to do the things necessary to make our clients successful. Ultimately, we know the pharmaceuticals we help develop change lives. To that end, we will continue to invest in the company and our employees. Whether we are tasked with finding new solid forms, characterizing your material, solving a development issue, or helping improve your chemical intellectual property - we want you to reach your goals. If we enable you to achieve milestones we're confident you'll recommend us to your colleagues - and that's really the highest compliment and measure of success we can ask for.

So on behalf of all of the employees at Triclinic Labs, thank you for ten amazing years! It's been thoroughly enjoyable and rewarding. We look forward to helping you meet your current and future drug development challenges.

Read our entire 10th Anniversary letter.

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Today, Triclinic Labs announced the installation of it’s fourth powder diffractometer. The Rigaku SmartLab is the newest and most novel high-resolution X-ray diffractometer (XRD) available today.

Triclinic’s new X-ray diffraction system features the HyPix-3000 high-energy-resolution multidimensional semiconductor detector that supports 0D, 1D and 2D measurement modes, allowing all applications to be handled with a single detector, eliminating the inconvenience of preparing and switching individual detectors for different applications. The HyPix-3000 detector can be used to obtain 2D powder diffraction patterns, which can be processed to deliver superior qualitative analysis by using all the 2D pattern information.

Rigaku’s HyPix-3000 is a next-generation two-dimensional semiconductor detector. One of the HyPix-3000’s unique features is its large active area of approximately 3000 mm² with a small pixel size of 100 μm², resulting in a detector with high spatial resolution. In addition, the HyPix-3000 is a single photon counting X-ray detector with a high-count rate of greater than 10 cps/pixel, a fast readout speed, and essentially no noise. “This system has incredible detection capabilities and combined with our proprietary signal-to-noise optimization algorithms and digital filters, this will enable unsurpassed sensitivity in routine sample analysis or method development” said Simon Bates Ph.D., Triclinic’ s Research Fellow and diffraction expert. The system incorporates a high-resolution Î./Î. closed loop goniometer drive system with an available in-plane diffraction arm. The system’s new Cross-Beam-Optics (CBO) family feature fully automated switchable reflection and transmission optics (CBO-Auto). The new system can be used for powder, liquid, film, and textile samples and allows mapping measurements within suitable samples.

For more information please contact sbates@TriclinicLabs.com

The new XRPD instrument is part of Triclinic's 2018 capital campaign for advanced instrumentation. Other instruments recently added include a 400 MHz NMR with solids and liquids capability, new thermal analysis instruments, particle size analysis, chromatography, and spectroscopic imaging (IR and LFR).

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In support of its Chemistry Manufacturing and Controls services including structure elucidation, method development, polymorph characterization, and problem solving, Triclinic Labs announced the successful installation of a state-of-the-art nuclear magnetic resonance (NMR) instrument with TopSpin acquisition and analysis software. The new system provides multi-dimensional liquids analysis with a broadband probe allowing for a myriad of experiments (1H, 13C, 15N, 31P, etc.). In addition, the system is configured with 4 mm magic angle spinning probe and associated high-power amplifiers for broadband solid-state NMR analysis. “We’re pleased to add this extremely flexible instrument to our laboratory and in support of our analytical chemists” said David Bugay, Ph.D., Triclinic’s Chief Scientific Officer. “ We’ve already begun qualification of the instrument and expect that it will be cGMP compliant soon. We’ll offer non-cGMP analyses until then” he added. In addition to the new instrument, Triclinic has added third party NMR software to be utilized by three Ph.D.s with extensive NMR interpretation skills. “Aeri Park, Pat Stahly, and I have spent the better part of the last three decades interpreting and analyzing organic materials using multi-dimensional liquids and solid-state NMR spectroscopy. It will be of great benefit in terms of time and data quality for our clients to have that capability in house” Bugay said. The new instrument is part of Triclinic’s 2018 capital campaign which also will add a third Rigaku X-ray powder diffractometer, additional liquid chromatography, and several advanced spectroscopic capabilities.

For more information, please contact Triclinic Labs. RFI@TriclinicLabs.com

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In support of its materials analysis and patent prosecution / litigation support groups, Triclinic has added two separation systems. A latest generation Agilent Infinity II 1260 HPLC system and a Thermo Fisher Trace 1310 GC with Headspace capabilities. The 1260 UPLC-HPLC system is equipped with a diode array detector and a quaternary pump. The quaternary pumping system provides added flexibility by allowing a scientist to utilize and mix up to four (4) different solvents at the same time reducing development time while at the same time aiding accuracy and precision of methods. "The new Agilent 1260 systems offer added sensitivity and functionality for identification, assay and impurity method development and validation “said Dr. Aeri Park, Vice president at Triclinic Labs. “We have added a gas chromatography system to add capabilities in residual solvent analysis” she added. Â A GC is Used for analyzing compounds that can be vaporized without decomposition. Typical uses of GC include identification, purity / impurity analysis, and for cGMP testing per compendial methods.

The new chromatography instruments are part of Triclinic’s 2018 capital campaign.

For more information, please contact Triclinic Labs. RFI@TriclinicLabs.com

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G. Patrick Stahly, Ph.D., COO of Triclinic Labs, will present an overview of the importance of solid state in the pharmaceutical development process during his talk " Current trends in pharmaceutical solid-state chemistry." A discussion of the newest tools utilized to improve API solid properties as well as patent application strategies to protect solid forms will be presented.

2018 BPCR Conference Biotech, Pharma, Cancer, and Research Conference August 29, 2018 Purdue Research Park, West Lafayette, IN

For more info please visit: https://www.bpcrconference.com/

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Triclinic Labs, Inc. welcomes Dr. Andy Gilkison as our new Scientific Director. Dr. Gilkison received his Ph.D. in Physical Chemistry from Purdue University in 2005, where his research focused on the investigation of intra molecular relaxation dynamics in super-excited states of small molecules using muli-resonance optical spectroscopy. Dr. Gilkison spent 9 years, prior to joining Triclinic Labs, as a research Investigator at SSCI, Inc., where he later advanced to the position of Senior Research Investigator. There he served as a subject matter expert for vibrational spectroscopy, and developed and validated GMP solid state analytical methods for pharmaceuticals. At Triclinic, Dr. Gilkison will help expand method development and validation as well as involvement in analytical projects, and evaluation of new instrumentation. “Honestly, I think I am the most excited about the fact that Triclinic Labs is so interested in both science as well as being an industry leader in solid-state development” Dr. Gilkison commented. “For example, most of the equipment here is new and cutting edge and that’s exciting to me. It is not just a simple contract lab, it’s the people here that are very engaged in what they do. They are very passionate and want to be the best, and they can do that with the technology they have” he continued.

“We’re pleased to hire someone of Andy’s, experience and knowledge” said David Bugay Ph.D., Triclinic’s CSO. “He brings a wealth of ideas and approaches to drug substance and drug product analysis which greatly strengthens Triclinic’s capabilities” he continued. To contact Andy Gilkison, you may email him at AGilkison@TriclinicLabs.com or phone at +1.765.588.5634. For more information on how Triclinic Labs can help strategically position your solid-state pharmaceutical programs for success using the most innovative development and analysis tools, please request a free consultation by clicking here.

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Triclinic Labs, Inc. announced it has added a Thermo Infrared Imaging Microscope to its extensive suite of drug product and chemical imaging instruments. A state-of-the-art Nicolet iN10 MX Imaging Microscope and Infrared imaging system for drug substance and drug product analysis was purchased. The microscope and imaging system, offer the power required to rapidly acquire and analyze chemical images to enhance understanding of the chemical distribution of materials in heterogeneous samples. "With this system we can analyze samples as small as 50 microns with no liquid nitrogen using a standard room temperature detector. We have Spatial resolution better than 10 microns" said Dave Bugay, Ph.D. Triclinic's CSO. "This adds to our comprehensive suite of imaging and mapping systems which Triclinic uses for counterfeit, infringement, and contaminant analyses" he continued. For more information, please contact DBugay@TriclinicLabs.com

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Triclinic Labs, Inc. announced Dr. Aeri Park has joined its contract solid-state pharmaceutical development group as Vice President. Dr. Park received her Ph.D. from the University of Oklahoma and is a recognized industry expert in API solid form screening and selection, solid-state characterization of APIs, intermediates, and drug products, crystallization method development, patent prosecution support, and frequently acts as an expert witness in Paragraph IV litigation matters both domestically and internationally. Dr. Park will lead Triclinic’s efforts in physical and analytical chemistry services as well as contribute to its patent prosecution and litigation expert services practice. Dr. Aeri Park, was formerly Director of US Operations for Almac Group and established and grew a US-based analytical laboratory for the firm. Prior to joining Almac, Dr. Park was instrumental in the growth and scientific success of SSCI, a solid-state development group. “I’m excited to return to solid-state research and development with Triclinic Labs” Dr. Park commented. “I have worked with most of the scientists and staff here before and I am excited at the level of interpretation and innovation they bring to not only solid form screening and selection but also solids materials characterization and method development. It’s well beyond anything I’ve seen at other companies and it’s very exciting to see what it offers clients” she continued. “We are fortunate to attract someone’s of Aeri’s reputation and accomplishment in solid-state pharmaceutical sciences. We feel Triclinic can fully leverage her expertise and apply it to the novel approaches and techniques we’ve developed and continue to innovate in” said Dr. David Bugay, Triclinic’s Chief Scientific Officer.

To contact Aeri Park you may email her at APark@TriclinicLabs.com or phone at +1.765.588.9538.

For more information on how Triclinic Labs can help strategically position your solid-state pharmaceutical programs for success using the most innovative development and analysis tools, please request a free consultation by clicking here.

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Cocrystals: A Regulatory Rebirth Pat Stahly, Ph.D.

What is the impact of recent changes in FDA guidance on regulatory and intellectual property issues?

The FDA reclassification of cocrystals as active pharmaceutical ingredients (APIs) has created exciting opportunities for the pharmaceutical industry. That reclassification means cocrystals can now be developed as if they were polymorphs, providing new avenues for dealing with poor API physical properties and extending intellectual property lifetimes. It is important to understand how the revised guideline impacts API development, regulatory submissions, and intellectual property protection. Those topics are discussed in this whitepaper. Also considered is the importance of identifying whether an API is a salt or a cocrystal, a critical classification from a regulatory point of view. In addition, a list of FDA-approved, marketed cocrystals is presented. Finally, recommendations for cocrystal screening, evaluation, formulation, and production at scale are given.

To download the complete cocrystal whitepaper please click here.

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Partnership will enable Novasep to offer early-stage solid-state chemistry services in North America

Lyon, France, Novasep, a leading supplier of services and technologies for the life sciences industry, today announces its partnership with Triclinic Labs, Inc., a US-based provider of contract pharmaceutical and fine chemical solid-state development services. This is Novasep’s first partnership agreement focusing on early-stage, solid-state services. Those services will be in addition to Novasep’s existing, early-stage, active pharmaceutical ingredient (API) synthesis and purification services and will be available to customers in North America as well as other regions.

The newly-formed alliance between Novasep and Triclinic Labs will enable both parties to serve their customers with full service development of APIs, from first chemical synthesis to solid form optimization. Novasep’s services will be extended to include solid form screening, selection, development, characterization, and analytical method development.

While the efficiency of a drug is based on its intrinsic nature and its interactions with biological targets, the preparation process has a strong impact on these properties. Finding the most appropriate solid phase can optimize these features. The best solid phase - be it a crystalline polymorph, salt, cocrystal, or amorphous form, can maximize physicochemical properties and therefore improve drug efficiency.

“This new partnership with Triclinic Labs is a further step in our ‘Back to Basics’ strategic plan. It enables us to expand our offering to our clients adding services on the last stage of product development,” said Dr. Michel Spagnol, CEO of Novasep.

“The alliance with Triclinic Labs emphasizes our continued commitment towards the North American market, following the recent opening of our US-based synthesis laboratory and kilo lab in Boothwyn, PA,” said Andrew Brennan, general manager at Novasep’s US operations.

“This alliance was designed from the ground up to benefit companies who want a seamless hand off between development and scale up. While there are numerous synthesis companies and early stage development groups, this alliance is distinctive as it pairs two leading companies with extensive, unique, and demonstrated physical and analytical chemistry capabilities” - said Dr. David Bugay, CSO of Triclinic Labs. “We can now offer world-class large and small molecule screening, characterization, purification, control, scale up, method development/validation, and intellectual property support capabilities.”

“The exciting thing about this strategic alliance is there is real commitment and effort behind it at all levels of both companies.” Shawn Comella, Triclinic Labs’ CEO commented. “We believe that collaboration will lead to increased efficiency and success for our clients when they require both solid-state development as well as API manufacturing expertise.”

About Novasep Novasep is a global provider of cost-effective and sustainable manufacturing solutions for life sciences molecules and fine chemicals. Novasep's unique offering includes process development services, purification equipment and turnkey processes, contract manufacturing services and complex active molecules to serve pharmaceutical, biopharmaceutical, fine chemical, food and functional ingredients as well as fermentation and chemical commodities industries.

https://www.novasep.com

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Triclinic Labs opened its new, custom built research facilities today. The 18,000 square foot complex houses extensive physical and analytical chemistry laboratories, controlled room temperature and stability facilities, and office and conference spaces. Nearly two years of planning and construction went into the new facility. "The new space was designed to not only provide optimal work-flow and efficiency but also was engineered specifically with pharmaceutical development and testing in mind. We're extremely pleased with its functionality" said Shawn Comella, Triclinic's CEO. "The building has extensive climate control and air handling functions as well as a central facilities hub and individual laboratories to serve as both cGMP and non-GMP workspaces," he continued. With the opening of the new facility, Triclinic Labs doubled its footprint and research services capacity. In addition to the new facility, Triclinic invested heavily in new capital equipment including a third X-ray powder diffractometer, digital microscopy, and additional chromatography systems to meet client demands.

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Today Triclinic Labs announced it will significantly expand its business development team to meet increasing demand for its services. The additions include personnel and regional expansion. "The requests for our unique offerings as well as our trusted physical and analytical chemistry services have grown beyond our expectations" said Shawn Comella, Triclinic's CEO. "We are adding capacity to meet the rapid response and exceptional service standards we set at the founding of the company and our clients have come to expect," he added. The new capacity will allow Triclinic to meet the rapidly growing US and European demand for its solid state analytical and development services. The team will also assess the regular licensing, research and development, and co-development opportunities it receives. "We believe we can do more to help emerging companies move their compounds toward the clinic - but one of the hardest parts of doing that is assessing the opportunities in a timely and triaged manner," said Dr. Pat Stahly, Triclinic's COO. "This added capacity will allow us to quickly respond to that potential and determine if it's mutually beneficial." To apply for a business development position please visit our employment page here . For more information on Triclinic Labs, please contact us here .

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Today Triclinic Labs announced it has implemented a new VHX series digital imaging system from Keyence for use in litigation support, contaminant analysis, and analytical chemistry projects. “The VHX Series was designed to overcome the limitations of traditional optical microscopes by providing high-resolution, large depth-of-field imaging and integrated 2D/3D measurement in a system and offers the highest frame rate digital microscope camera in the industry,” said David Bugay, Ph.D. Triclinic’s CSO.

The system offers a magnification range from 0.1x - 5000x and the VHX Series enables a wide range of microscopic observation from macro-scale stereoscopic imaging to the detailed analysis of an SEM. Many lighting techniques are also supported including bright and dark field, transmitted, polarized, and differential interference observation. “The system uses short-wavelength light and pixel shift technology to improve resolution by up to 25%. Now we can image any object in sharp contrast and detail,” said Michael DeLion, Senior Analytical Scientist and at Triclinic.

For more information about Triclinic Labs’ Digital Imaging capabilities please click here.

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Variable temperature and/or variable humidity (VT/VH) in situ analysis is an important technique in solid-state pharmaceutical development as it allows one to probe dynamic conversions between a variety of crystalline and non-crystalline API systems. A VT/VH system also permits quantification of multiple solid phases.

Triclinic Labs today installed a custom built, computer controlled, VT/VH environment stage that may be used not only for transmission X-ray diffraction (XRD) but can also be mounted on the company’s dispersive Raman instrument, and optical microscopy stages. “A good working knowledge of active pharmaceutical ingredient kinetic, thermodynamic, and thermal behavior is critical for successful development,” said Dr. Simon Bates who led the system’s development.

“VT-XRD can provide incredible information with regard to crystal structure, phase transitions, decomposition, crystallization, and thermal events of pharmaceutical ingredients,” he added. “The true power of this system is in its flexibility,” said Dr. David Bugay, Triclinic’s CSO. “Not only can we analyze the same sample using multiple techniques like transmission XRD and Raman spectroscopy at variable temperatures and humidity, but also correlate that information with thermal data using chemometrics for the most detailed understanding of complex systems,” he continued.

For more information on Triclinic Lab’s variable temperature/environmental in situ analysis capabilities please contact us by clicking here.

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Dr. Scott Childs, Vice President of Chemistry at Triclinic Labs, announced that the article "Formulation of a Danazol Cocrystal with Controlled Supersaturation Plays an Essential Role in Improving Bioavailability" was recently published in the peer-reviewed journal, Molecular Pharmaceutics. In the paper Dr. Childs demonstrates the bioavailability of the newly formulated danazol cocrystal increased by over 10 times compared to the poorly soluble danazol polymorph. Dr. Childs said "This is the first systematic investigation of a supersaturating cocrystal system where the goal was to simultaneously consider both the solid form and the formulation in order to generate commercially and therapeutically relevant blood levels in pharmacokinetic studies. It is believed that these results are generally applicable to cocrystals of poorly soluble APIs and cocrystals that are formulated as designed supersaturating systems will consistently show higher bioavailability and a higher percent of the dose absorbed." The publication on cocrystals, their formulation, and subsequent dramatic improvement in bioavailability is available by clicking on this link.

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Simon Bates, Ph.D. announced Triclinic's collaboration with Steven Nail, Ph.D. and Baxter Pharmaceutical Solutions has led to the publication of new methods for the analysis of residual water content in lyophile cakes. "Total X-Ray Powder Diffraction Analysis (TXRPD) using transmission geometry was able to observe significant variance in measured powder patterns for sucrose lyophilzates with differing residual water contents. Integrated diffraction intensity corresponding to the observed variances was found to be linearly correlated to residual water content as measured by an independent technique." Bates said. The team observed variance was concentrated in two distinct regions of the lyophilizate powder pattern, corresponding to the characteristic sucrose matrix double halo and the high angle diffuse region normally associated with free-water. Full pattern fitting of the lyophilizate powder patterns suggested that the high angle variance was better described by the characteristic diffraction profile of a concentrated sucrose:water system rather than by the free-water diffraction profile. This suggests that the residual water in the sucrose lyophilizates is intimately mixed at the molecular level with sucrose molecules forming a liquid/solid solution. The bound nature of the residual water and its impact on the sucrose matrix gives an enhanced diffraction response of between 3.0 and 3.5 beyond that expected for free-water. The enhanced diffraction response allows semi-quantitative analysis of residual water contents within the studied sucrose lyophilizates to levels below 1% by weight.

"This approach should allow for much better tuning of the lyophilization process and offers an analytical tool to improve development results and time" Bates said.

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Pat Stahly, Ph.D., Triclinic's Chief Operating Officer, announced today that David Jonaitis has been promoted to Scientific Director within the Chemistry Group. "Dave is an exceptional scientist, both in his ability to execute complex projects as well as creatively develop new approaches to solving solid-state development issues. He very much deserves this promotion" said Dr. Stahly. Jonaitis has been employed at Triclinic since 2011 and has taken on increasing responsibilities since joining the company.

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Brandi Albea, Director of Quality Systems at Triclinic Labs announced the company has received its registration certification from the US Food and Drug Administration (USFDA). "We're pleased to now offer cGMP method development and routine testing services for our pharmaceutical clients" Ms. Albea said. The services were implemented to support Triclinic's clients who have requested lot release and method testing for production environments. "We've invested heavily in the infrastructure and personnel to make this a very flexible system while at the same time fully complying with the USFDA regulations for cGMP." Ms. Albea said. "The system is unique and should result in lower costs and a much more responsive time-line for testing and method validation." she said.

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In x-ray powder diffraction, the 2theta. positions of diffraction peaks are directly proportional to the wavelength of the incoming x-rays (λ) according to the Bragg equation: n(Lambda)=2dsinÎ.Â.. Longer x-ray wavelengths result in greater 2theta. positions. That allows observation of low-angle peaks that are not observable using shorter wavelength x-rays and provides better peak separation. Triclinic Lab’s Rigaku Smart-Lab system is typically configured with a copper source, providing x-rays with a wavelength of 1.54 Ã…. However, for some analyses a cobalt source, providing x-rays with a wavelength of 1.79 Ã, is used. The higher diffraction angles and peak spreads from the cobalt source can allow differentiation of samples when the Cu might not. Triclinic announced that it has acquired a Co source for use in routine polymorph, salt, and cocrystal screens. "The addition of a Cobalt x-ray source gives us a powerful tool in the tool box for drug substance solid-form differentiation." said Dr. Pat Stahly, Triclinic's COO. Download the Whitepaper entitled " Advantages of a Cu vs. Co X-ray Diffraction Source" - By Pat Stahly - Triclinic Labs -Q32012

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Today, Triclinic Labs, Inc., announced the creation of a new, ultra rapid turn-around X-ray Powder Diffraction analysis service. Samples received by 12 pm EST will receive results by 12 pm EST the following day at no extra charge! Online submission and data reporting is available and is included in the $250 per sample charge. Interpretive reports are also available for an additional charge. This service is non-cGMP. "We believe that our 24 hour EXpress XRPD service sets a precedent in the solid-state service industry for turnaround and value." said Shawn Comella, Triclinic's CEO. "Providing a straightforward, rapid service, with exceptional analytical high quality gives our client base an option to further improve their development resources" he added. For more details on Triclinic Labs' 24 Hour XRPD/XRD Analysis Services, please click here.

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