Analytical Studies


  • Test article characterization and stability studies
  • Dosing formulation stability and homogeneity studies
  • Plasma drug concentration measurement using LC-MS/MS

We can now conduct TK and PK measurements using LC-MS/MS, not only at our Pharmacokinetic and Bioanalysis Center in Wakayama, but also on-site at our Drug Safety Research Laboratories in Kagoshima.


Tests and Assays Offered

  • Chloride limit test
  • Flame coloration test
  • Heavy metal test
  • Qualitative tests
  • Arsenic limit test
  • Liquid chromatography
  • Gas chromatography
  • Thin-layer chromatography
  • Fluorometry
  • Spectrophotometry
  • Amino acid analysis
  • Carbohydrate analysis
  • Infrared spectrophotometry
  • Loss on drying
  • Freezing point determination
  • Loss on ignition
  • Residue on ignition
  • Residual solvents
  • Osmolarity determination
  • Water determination (Karl Fischer Method)
  • Optical rotation
  • Titrimetry
  • Peptide analysis
  • Aluminum analysis
  • Specific gravity and density
  • pH measurement
  • Melting point determination
  • Particle size determination (sieve method)
  • Endotoxin test
  • Pyrogen test
  • Sterility test
  • Insoluble particulate matter test for injections
  • Disintegration test
  • Properties
  • Protein measurement

Examples of dosage forms handled

Active pharmaceutical ingredients, solutions, granules, eye ointments, suspensions, emulsions, suppositories,

powders, tablets, injections, patches, eye drops, ointments,

vaccines

 

Characterization and Stability Studies

Typical measurement parameters

  • Physical properties
  • Identification (FTIR)
  • Purity and content assays (HPLC)
  • Water determination (Karl Fischer Method method)

Time to completion: 4 weeks (COA within 3 weeks)

 

Validation of Characterization Methods (for purity and assay tests using HPLC)

Typical measurement parameters

  • Specificity
  • Linearity
  • Stability in autosampler
  • Repeatability

Time to completion: 4 weeks

 

Validation of Dose Formulation Concentration Method

Typical measurement parameters

  • Specificity
  • Linearity
  • Stability in autosampler
  • Accuracy and repeatability
  • Intermediate precision

Time to completion: 4 weeks

 

 

Fourier Transform Infrared Spectroscopy (FTIR)

 

Identification Test

Equipment: FTIR (Fourier transform infrared spectrophotometer)

Manufacturer: Shimadzu Model: FTIR-8400

Advantages:

  • Potassium bromide (KBr) tablet method
  • Potassium chloride (KCl) tablet method
  • ATR method: Using the ATR method, the sample can be measured without compression or pretreatment.

Advantages:

  • There is limited variation because there is no need to prepare the samples.
  • Accuracy is high, and trace amounts can be measured. There are also no ion exchange reactions.

 

FTIR
FTIR
KBr method  (P- Hydroxypropylbenzoate) Measuring time: about 1 hour
KBr method  (P- Hydroxypropylbenzoate) Measuring time: about 1 hour
ATR method  (P- Hydroxypropylbenzoate) Measuring time: about 15 minutes
ATR method  (P- Hydroxypropylbenzoate) Measuring time: about 15 minutes

Ultra High Performance Liquid Chromatography

Purity, assay

Equipment: UHPLC (Ultra High Performance Liquid Chromatograph)

Manufacturer: Shimadzu Models: 20A, 30A 

Advantages:

  • Shortened run times and high sample throughput
  • Ideal for measuring samples with limited stability
  • or long measurement times

Approximately 1/4 to 1/5 reduction in run times Amino acid measurement (Standard solution mixture, PTC derivitization)
Approximately 1/4 to 1/5 reduction in run times Amino acid measurement (Standard solution mixture, PTC derivitization)

Water determination (Karl Fischer Method)

 

Moisture content

Equipment: Moisture titrator

Manufacturer: Kyoto Electronics Manufacturing

Type:

  • Volumetric titration method Karl Fischer Method moisture meter (MKA-510)
  • Coulometric titration method Karl Fischer Method moisture meter (MKC-510N)

Advantages:

  • Controlled by dedicated software (KF-Win / ER).
  • Suitable for measuring very small samples and samples with high hygroscopicity by using a specific sample cup and MKA-510 MKC-510N  sample input device.
MKA-510
MKA-510
MKC-510N
MKC-510N
Sample input device
Sample input device

Ion chromatographic method

 

Ion analysis, amino acid analysis

Equipment: Ion chromatograph (IC)

Manufacturer: Thermo Fisher Scientific Model: ICS-3000

Advantages:

  • Capable of high sensitivity measurement for various ions, sugars, and amino acids.

Trifluoroacetic acid measurement (residual solvent)

Even with an injection volume of 1/3, the limit of quantification is 4 times lower.

Shimadzu 10A + CDD10A (Non-suppressor system) Injection volume: 300 micro L Limit of quantification: 0.1 micro g/mL
Shimadzu 10A + CDD10A (Non-suppressor system) Injection volume: 300 micro L Limit of quantification: 0.1 micro g/mL
ICS-3000 + CDD (Suppressor system) Injection volume: 100 micro L Limit of quantification: 0.025 micro g/mL
ICS-3000 + CDD (Suppressor system) Injection volume: 100 micro L Limit of quantification: 0.025 micro g/mL

Stability Studies

Samples are stored at the specified conditions, and the test items are conducted at each time point.

 

Samples

Active pharmaceutical ingredients, solutions, granules, eye ointments, suspensions, emulsions, plasters, suppositories, tablets, injections, eye drops, ointments.

 

Storage Capabilities

Storage Equipment

Performance

Temperature ranges

Humidity ranges

Temperature and humidity controlled cabinets

5 to to 85°C

40 to 95

-20 to 100°C

30 to 98

 

 

Storage rooms

Temperature ranges

Humidity ranges

Ordinary temperature room

15 to 25°C

80%

Refrigeration room

2 to C

-

Freezer room

-30 to -10°C

-


 

LC-MS/MS method

API4000 LC-MS / MS system: 3 instruments

Triple Quad 6500 LC-MS/MS system: 2 instruments