Triclinic Labs is capable of quickly and cost effectively analyzing solid form chemical samples using state-of-the-art instruments and techniques.
Whether you require simple analysis for identification, more extensive interpretation of analytical data or development of analytical methods, we have the experience and techniques to meet your needs. Most services are executd with 24-48 hour turnaound at no extra cost. We will provide you with a quote for any of the services listed. Please see below.
API and Drug Product Characterization
The Chemical, Manufacturing, and Control (CMC) section of New Drug Applications (INDs) and Abbreviated New Drug Applications (ANDAs) is required to contain complete chemical and physical characterization of an API. Triclinic can help you gather and interpret all the data needed for a CMC section.
We have experience with the necessary analytical techniques and their use in both qualitative and quantitative modes. These techniques include NMR spectroscopy (solution and solid), mass spectrometry, infrared and Raman spectroscopy, X-ray diffraction analyses (powder and single-crystal), differential scanning calorimetry, thermogravimetry, microscopy, dynamic vapor sorption, particle sizing, and others.
We also have experience determining properties such as solubility, dissolution rate, hygroscopicity, water-organic partition behavior, relative thermodynamic stability, etc. In addition, Triclinic can guide you through the development and validation of quantitative analytical methods to be applied to solid mixtures.
Triclinic can help you with drug product issues such as verifying API polymorphic form throughout drug product manufacture, out-of-specification troubleshooting, and development and validation of analytical methods.
We are well versed in:
- Rapid Diffraction, Spectroscopic, Microscopic, and Thermal Analysis of Drug Substances and Drug Products
- Characterization and Identification of Polymorphs in Drug Substances and Products
- Deviation Analysis
- Failures, OOS, Contaminants
- Failures, OOS, Contaminants
- Content and Blend Uniformity
- Distribution
- Domain Analysis
- Intellectual Property Support
- Analysis of Controlled Release Systems
- Content Uniformity
- Degradation
- Drug Migration/ Ingress/ Egress
- Drug Product & Medical Device (e.g. Stents)
- Failure Analysis
- Ingredient-Specific Particle Size
- Intellectual Property Support
- Layer Thickness
- Polymorph Analysis
- Particle Characterization
- Aggregation and Agglomeration Studies
- Ingredient-Specific Particle Shape
- Ingredient-Specific Particle Size Distribution
- Particle Interaction
Instrument and Technique List (click on a Technique Name for a Wiki Description of peformance)
Traditional Small Molecule/Physical & Chemical Characterization |
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Technique |
Brand |
Model |
Notes |
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Digital |
AFM |
All modes |
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| Micro Calorimetry | MicroCal/GE | ITC 200 | ||
DSC |
TA Instruments |
2920 |
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Dynamic Vapor Sorption |
VTI |
SGA-100 Q5000SA |
Range of %RH ( 15-100) Range of %RH (5-100) |
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Contact Angle Apparatus |
Ramehart Imaging System |
NA |
Drop Image Advanced Software Version 1.4.11 |
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FT-IR |
Thermo |
Nicolet 6700 |
ATR, diffuse reflectance, transmission, gas cell, spectral libraries |
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Dissolution |
Van Kel |
VK 7000 |
UV/VIS or HPLC detection |
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Disintegration Tester |
Van Kel |
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Hot Stage Optical Microscopy |
Linkam |
LTS420 |
Ambient – 600 °C |
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HPLC |
Agilent |
1100 |
Detectors: diode array, refractive, light scattering |
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Inverse Gas Chromatography |
Surface Measurement Systems, U.K |
NA |
Ambient – 200 °C |
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Karl Fisher |
KF |
NA |
All modes |
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Mass Spectrometry |
Voyager |
DE Pro |
GC/MS, LC/MS, LC/MS/MS and MALDI |
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Microtome |
Leitz |
Rotary |
Tungsten-Carbide, stainless steel, and Diamond Blades |
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Microtome |
MTX |
Ultramicrotome |
Tungsten-Carbide and Diamond Blades |
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NMR |
Bruker |
400/500/600/800 MHz |
Liquids, multi-nuclear |
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NMR |
Bruker |
400 MHz |
Solids, multi-nuclear |
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Optical Microscopy |
Leica |
M80 - Stereo |
Still and dynamic image capturing |
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Optical Microscopy |
Leica |
DM2500P - Compound |
Still and dynamic image capturing |
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Particle Charge |
Faraday Pail |
NA |
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Particle Size |
CILAS |
1180 LPSA |
Laser diffraction system, interfaced to microscope for real time laser diffraction/optical analysis, optical microscopy image analysis also available |
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Particle Size |
HIAC/Royco |
3000 |
Light obscuration |
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Powder Tester |
Revolution |
NA |
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RAMAN |
Renishaw Dispersive |
inVia |
Chemical imaging, microsampling, Confocal, 785 nm laser |
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RAMAN |
Thermo FT |
Module |
Micro and macro sampling, 1064 nm laser, spectral libraries |
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SAXS |
Rigaku |
SmartLab-2010 |
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Scanning Electron Microscopy |
FEI |
NOVA nanoSEM FE |
High resolution imaging, cryo capabilities, environmental SEM |
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SEM/Energy Dispersive X-Ray |
Above |
NA |
Micro-elemental analysis, mapping |
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Single Crystal X-Ray Diffraction |
Rigaku |
Rapid II |
Structure determination, absolute configuration |
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Surface Analyzer |
MSE |
396 |
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Tablet Hardness |
Van Kel |
NA |
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Texture Analyzer |
TA |
XT2 |
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TGA |
TA Instruments |
2050 |
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PerkinElmer |
Lambda 25 |
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Rigaku |
SmartLab-2010 |
Powders, Tablets, Mapping, Transmission |
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SCINTAG |
X1 |
Fully configurable parameters |
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Diffractometry, Spectroscopy, Microscopy, Thermal Analysis
Characterization of solids involves multiple analytical techniques, all of which are second nature to the staff of Triclinic. X-ray diffractometry is a primary technique, directly probing the intermolecular arrangements of molecules in solids. In most cases, a powder x-ray diffraction pattern is the best "fingerprint" of a solid form.
Vibrational spectroscopy, although a secondary technique, is nevertheless of tremendous importance in solids analysis. Intermolecular interactions affect covalent bond vibrational frequencies, which are detected using infrared or Raman spectroscopy. Solid-state NMR spectroscopy is quite useful for solids characterization. Also a secondary technique, it probes the electronic environments of atoms, which are influenced by intermolecular interactions. In addition to standard characterization applications, spectroscopic techniques are particularly useful for quantitative solid mixture analysis.
Microscopy is the oldest, and perhaps recently the most neglected, of the solids characterization techniques. Thermal microscopy was used by Kofler and others to identify polymorphs and cocrystals before diffractometry and spectroscopy were commonplace. A lot can be accomplished with microscopy, using very little material.
Thermal analytical techniques are differential scanning calorimetry (DSC) and thermogravimetry (TG). Characterization data obtained include melting and phase transition temperatures. For non-crystalline solids, glass transition temperatures can be determined. The combination of DSC and TG is particularly useful for identification of hydrates and solvates.
To obtain analysis please submit sample requests electronically or manually (click here).
To obtain a quote for analytical services - please click here.
Small Scale Formulation Equipment |
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Technique |
Brand |
Model |
Notes |
Ball Mill |
Retsch |
Brinkman |
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Beta Tablet Press |
Manesty |
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Blender |
Hobart |
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Comil |
Retsch |
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Cyro Mill |
Spex CertiPrep 6750 |
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Low temperature milling operation |
Extruder |
Friji Paudal |
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Fluid Bed Dryer |
Glatt |
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Fluid Bed Dryer |
Vector |
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Granulator |
Hobart |
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Low shear |
Lyophilizer |
Lyo-Star |
FTS |
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Mill |
Fitzpatrick |
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Mill |
Stokes |
M6 |
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Roller Compactor |
Fitzpatrick |
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Rotary Sample Divider |
Retsch |
PT100 |
Representative sampling for powders |
Spheronizer |
Friji Paudal |
QJ-230T |
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Spinning Riffler |
Retsch |
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Spray Dryer |
Yamato DL-410 |
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Aqueous spray dryer; Buchi –B290 (solvent) limit availability |
Tablet Press |
Korsch |
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Tablet Press |
Stokes |
B2 |
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V-Blender |
Retsch |
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Wet Granulator |
Key |
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5Kg capacity |
Wet Granulator |
Diosna |
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4Kg capacity |
To obtain analysis please submit sample requests electronically or manually (click here).
To obtain a quote for analytical services - please click here.
Bioanalytical Characterization |
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Technique |
Brand |
Model |
Notes |
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Amino Acid Composition Analysis |
Thermo/ABI |
OrbiTrap |
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Analytical Ultracentrifugation |
Beckman Coulter |
XLA/XLI |
Sedimentation velocity and equilibrium |
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Classical Light Scattering |
Wyatt |
MiniDawn-TREOS/OptiLab-T-rEX |
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Circular Dichroism |
Jasco |
J-815 |
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HPLC |
Agilent |
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SEC-HPLC |
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| Post-Translation Modification Analysis | LC/MS Above |
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Peptide Mapping (LC/MS/MS) |
LC/MS Above |
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ESI and MALDI |
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Surface Plasmon Resonance |
Biacore |
3000 |
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To obtain analysis please submit sample requests electronically or manually (click here).
To obtain a quote for analytical services - please click here.
Other Services Available |
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Technique |
Brand |
Model |
Notes |
ICP-MS |
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ToF-SIMS |
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XRF |
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Maximum Data from X-ray Powder Diffraction
XRPD data can be much more useful than just providing a phase fingerprint... to get the most from XRPD one needs an XRPD instrument, appropriate software, and technical expertise. The first two are readily available but the last is harder to come by.
Currently at Triclinic, we have a fully configurable- Scintag diffractometer, a state-of-the-art Rigaku SmartLab System, and a world-class, in-house technical expert. These capabilities allow us to extract much more information from an XRPD pattern than simply a finger-print identification. For example, we can index a powder pattern to determine the dimensions of the unit cell from XRPD data (vs. requiring synchrotron data). This requires accurate data, sophisticated software, and expert interpretation of the data. With the open design, configurable Scintag diffractometer it is possible to collect indexable powder patterns from small amounts of pharmaceutical materials (e.g. 10 mg of acetaminophen).
An indexed pattern can provide:
- Assurance of phase purity
- Identification of a phase as a probable hydrate or solvate based on unit cell void space
- Efficient pattern matching (in screening, for example) based on expected peak positions calculated from the unit cell
- Improved knowledge that can make up for poor-quality data resulting from small sample sizes Investigation of process-induced product changes leading to XRPD changes
- Understanding that a "new peak" showing up in the XRPD pattern of a material produced using a commercial process can be a symmetry-disallowed peak that arises because of defects rather than being a peak from a contaminant
- Excellent method to develop solid mixture quantitative analysis
Figure 1. Use of XRPD for determination of polymorphic conversion: a waterfall plot of XRPD patterns is shown for an API which has been subjected to different environmental conditions (temperature, relative humidity, time). Variations in peak intensity are noted for peaks at 18.6, 18.8, 19.8, 21.2, 21.5, and 22.8 Degrees 2Theta¸. The variations in peak intensities indicate the creation of a new polymorphic form of the API under the specified environmental conditions. This approach is useful for time-course studies under normal and modified conditions (e.g. stability, scale-up, formulation) to determine if polymorphic change arises. Infringement determination cases and process control experiments benefit from this approach as well
Single Crystal Growth and Structure Determination
Triclinic is not only able to obtain the unit cell of a crystalline solid phase but also is able to grow crystals suitable for single crystal studies if you do not have them.
