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  • Development, validation and comparison of two microextraction techniques for the rapid and sensitive determination of pregabalin in urine and pharmaceutical formulations after ethyl chloroformate derivatization followed by gas chromatography-mass spectrometric analysis.

Development, validation and comparison of two microextraction techniques for the rapid and sensitive determination of pregabalin in urine and pharmaceutical formulations after ethyl chloroformate derivatization followed by gas chromatography-mass spectrometric analysis.

Journal of pharmaceutical and biomedical analysis (2012-06-09)
Mohana Krishna Reddy Mudiam, Abhishek Chauhan, Rajeev Jain, Ratnasekhar Ch, Ghizal Fatima, Ekta Malhotra, R C Murthy
ABSTRACT

The present article reports first time the use of solid-phase microextraction (SPME) and dispersive liquid-liquid microextraction (DLLME) to extract pregabalin (PRG) from urine and pharmaceutical formulations followed by GC-MS analysis after ethyl chloroformate (ECF) derivatization. PRG is an antiepileptic and analgesic drug, which is a structural analogue of γ-amino-butyric acid (GABA). It is approved by Food and Drug Administration (FDA) for the treatment of central nervous system (CNS) disorders and neuropathic pain. Initially PRG was derivatized with ECF in the presence of pyridine at room temperature for 30s. Experimental parameters were investigated for derivatization, SPME and DLLME conditions. The limit of detection (LOD) and limit of quantitation (LOQ) were found to be 0.019 μg/ml and 0.063 μg/ml for SPME and 0.022 μg/ml and 0.075 μg/ml for DLLME respectively. The percentage recovery, in case of SPME was in the range of 83-98% while for DLLME it is in the range of 84-98%. The intra and inter-day precisions were found to be less than 6%. The developed methods after ECF derivatization were found to be simple, fast, efficient and inexpensive. DLLME has several advantages like lesser extraction time and cost effectiveness as compared to SPME. The developed methods may find wide application for the routine determination of PRG in biological as well as in quality control samples of pharmaceutical formulations.

MATERIALS
Product Number
Brand
Product Description

Supelco
SPME Fiber Assembly Polydimethylsiloxane/Divinylbenzene (PDMS/DVB), df 65 μm(PDMS/DVB, needle size 24 ga, StableFlex, for use with autosampler
Supelco
SPME Fiber Assembly Polydimethylsiloxane/Divinylbenzene (PDMS/DVB), df 65 μm(PDMS/DVB, for use with autosampler, needle size 23 ga
Supelco
SPME Portable Field Sampler, coating PDMS/DVB
Supelco
SPME Fiber Assembly Polydimethylsiloxane/Divinylbenzene (PDMS/DVB), df 65 μm(PDMS/DVB, needle size 23 ga, PDMS/DVB StableFlex, for use with autosampler
Supelco
SPME Fiber Assembly Polydimethylsiloxane/Divinylbenzene (PDMS/DVB), fused silica fiber, df 65 μm(PDMS/DVB, for use with manual holder, needle size 23 ga
Supelco
SPME Fiber Assembly Polydimethylsiloxane/Divinylbenzene (PDMS/DVB), df 65 μm(PDMS/DVB, needle size 24 ga, StableFlex, for use with manual holder
Supelco
SPME Fiber Assembly Polydimethylsiloxane/Divinylbenzene (PDMS/DVB), df 65 μm(PDMS/DVB, needle size 24 ga, for use with manual holder
Sigma-Aldrich
Ethyl chloroformate, 97%
Sigma-Aldrich
Ethyl chloroformate, purum, ≥98.0% (GC)
Supelco
SPME Fiber Assembly Polydimethylsiloxane/Divinylbenzene (PDMS/DVB), df 65 μm(PDMS/DVB, needle size 24 ga, for use with autosampler
Supelco
SPME Fiber Assembly Polydimethylsiloxane/Divinylbenzene (PDMS/DVB), df 65 μm(PDMS/DVB, for use with autosampler, needle size 23 ga, metal alloy fiber