Analytical Services

Our services:

• Analytical Method Development & Validation Development and validation of analytical methods for Drugs, Pharmaceuticals, Excipients, Impurities, related substances, residual solvents, powdered samples, dissolution samples, Microbiological tests, bacterial endotoxins, trace metals, heavy metals including rare earth metals and catalyst residues by IP, USP, BP, EP, JP.

Instrumentation Techniques:

• Mass Spectrometric methods such as LC-MS/MS, GC-MS/MS and ICP-MS/MS
• Electrophoretic methods such as electrophoresis (Capillary and Gel)
• Thermal methods such as DSC, DTA, TGA
• X-ray methods such as X-Ray diffraction

Extractable and Leachable Studies:

• Identification and quantification of drug product leachable to the extent practicable and within certain defined analytical threshold parameters 
• Selection of Container Closure System (CCS) for dosage forms Migration study for impurities possibly migrating from Ink/Gum and other components
• Extractable and Leachable studies on rubber stoppers, Gaskets & O-rings, Containers (HDPE, LDPE, PP), plastic bags, glass vials, syringes, tubing & filter, injectable bags/vials, films, blister packs, laminated tubes, etc.
• Development and validation of identified leachable as per the requirements of customers 

Techniques used for Extractable and Leachable Studies:

• GC-HS-MS for the analysis of semi-volatile and volatile components
• LCMS for the analysis of non-volatile components
• ICPMS for analysis of elemental impurities

Scanning Electron Microscopy / SEM Testing 
SEM/EDX allows analysis of elemental composition along with morphology and topography study of particles. The SEMs at NISHKA come equipped with EDX (also known as EDS). When exposed to an electron beam, the X-Rays emitted by an atom are unique, corresponding to its atomic number. EDX makes it possible to identify the elemental composition and sub-atomic properties of a sample. SEM analysis combined with EDX can help obtain more information and utilize analysis techniques appropriate for a given sample. EDX combined with SEM can be efficient to identify and examine samples at extremely high magnifications.

Impurity Profiling (As per ICH Q3 D)

Organic Impurities:
Estimation of know, unknown, volatile and non volatime organic Impurities, which are arises from API, Drug product formulation, Intermediates, unintended by products and degradation products during the manufacturing process or during the storage of drug substances using HPLC, GC/MS, LC /MS
Determination of enantiomeric impurities using HPLC.
Estimation of genotoxic impurities at PPM or PPB levels using HPLC, GC, LC/MS and GC/MS

Inorganic Impurities:
Determination of inorganic/ elemental impurities rise from manufacturing process reagents such as ligands, Catalysts, metals derived from other stages of production and elements derived from materials used in filtration by ICP/MS.
Estimation of As, Cd, Hg, Pb, Sb, Sn, Bi, Ag, Mo, V, Cr, Ni, Mo, Mn, Cu, Pt, Pd, Ru, Rh, Os, and Ir, but not limited to, using ICP/MS as per USP<232> & <233> levels ranging from PPM to sub PPT levels.

Degradation Impurities:

• Identification and Determination of degradation products/Impurities using hypernated techniques (LC/MS/MS) and HPL
• Conducting of forced degradation studies as per ICH guidelines for the assessment of stability indicating behavior of the product under unfavorable conditions.
• Establishment of degradation pathways and reaction mechanisms to evaluate the intrinsic stability of the product.
• Development and validation of stability indicating methods as per USP/ ICH guidelines.