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
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DOI：
10.1016/j.jpba.2012.05.001
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发表时间：
2012-11-01
影响因子：
3.4
通讯作者：
Murthy, R. C.
中科院分区：
文献类型：
--
作者：
Mudiam, Mohana Krishna Reddy;Chauhan, Abhishek;Murthy, R. C.
本文首次采用固相微萃取（SPME）和分散液液微萃取（DLLME）技术从尿液和药物制剂中提取普瑞巴林（PRG），氯甲酸乙酯（ECF）衍生化后进行气相色谱-质谱分析。PRG是一种抗癫痫镇痛药物，是γ -氨基丁酸（GABA）的结构类似物。它被美国食品和药物管理局（FDA）批准用于治疗中枢神经系统（CNS）疾病和神经性疼痛。最初，PRG在吡啶存在下，在室温下用ECF衍生30s。研究了衍生化、SPME和DLLME条件的实验参数。SPME的检出限和定量限分别为0.019 μ g/ml和0.063 μ g/ml， DLLME的检出限和定量限分别为0.022 μ g/ml和0.075 μ g/ml。SPME的回收率在83 ~ 98%之间，DLLME的回收率在84 ~ 98%之间。日间和日间的精确度小于6%。经ECF衍生化后的方法简单、快速、高效、经济。与SPME相比，dlme具有几个优点，如更短的提取时间和成本效益。该方法可广泛应用于生物制剂和制剂质量控制样品中PRG的常规测定。(C) 2012 Elsevier B.V.版权所有
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 gamma-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 mu g/ml and 0.063 mu g/ml for SPME and 0.022 mu g/ml and 0.075 mu g/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. (C) 2012 Elsevier B.V. All rights reserved.