Automated in-tube solid-phase microextraction coupled with liquid chromatography-electrospray ionization mass spectrometry for the determination of selected benzodiazepines.
Automated in-tube solid-phase microextraction coupled with liquid chromatography-electrospray ionization mass spectrometry for the determination of selected benzodiazepines.
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DOI：
10.1093/jat/24.8.718
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发表时间：
2000-11
影响因子：
2.5
通讯作者：
Haodan Yuan;Zoltán Mester;H. Lord;Janusz Pawliszyn
中科院分区：
文献类型：
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作者：
Haodan Yuan;Zoltán Mester;H. Lord;Janusz Pawliszyn
建立了一种简便、快速、灵敏的同时测定缓冲溶液、尿液和血清中7种苯二氮卓类药物（地西泮、去甲地西泮、替马西泮、奥沙西泮、7-氨基氟硝西泮、N-去甲基氟硝西泮和氯硝西泮）的方法。管内固相微萃取是一种用于水样中有机化合物的萃取技术，它是通过反复的抽/排循环，将样品中的分析物直接萃取到开放的管状毛细管柱中。采用Supelco LC-18色谱柱，以甲醇/50 mM醋酸铵水溶液（60：40）为移动的相，在离子抑制反相条件下分离苯二氮卓类药物。最佳萃取条件为：以60 cm长的Supelco-Q plot毛细管柱为萃取毛细管，以0.3 mL/min的流速，在100 mM Tris-HCl（pH 8.5）中，以30 mL样品进行10个循环的萃取。通过选择离子监测（SIM）模式进行定量研究。标准曲线在0.5 ng/mL或2 ng/mL至500 ng/mL范围内呈线性。方法的检出限为0.02 ~ 2 ng/mL。在优化的毛细管和裂解器电压下，每种化合物的特征离子在光谱中清楚地显示出来，并且可以使用LC-MS来鉴定这些化合物。该方法用于生物样品的分析，无干扰峰。然而，血清样品中的一些化合物的回收率需要进一步提高。
A simple, rapid, and sensitive method, which allowed us to simultaneously determine seven benzodiazepines (diazepam, nordiazepam, temazepam, oxazepam, 7-aminoflunitrazepam, N-desmethylflunitrazepam, and clonazepam) in buffer solution and in urine and serum samples, was investigated by automated in-tube solid-phase microextraction (SPME) coupled with liquid chromatography-electrospray ionization mass spectrometry (LC-ESI-MS). In-tube SPME, in which the analytes were extracted from the sample directly into an open tubular capillary column by repeated draw/eject cycles of sample solution, is an extraction technique for organic compounds in aqueous samples. The separation of benzodiazepines was carried out under ion-suppressed reversed-phase conditions by using methanol/50mM ammonium acetate in water (60:40) as a mobile phase with a Supelco LC-18 column. The optimal extraction condition was 10 draw/eject cycles of 30 mL of sample in 100mM Tris-HCl (pH 8.5) at a flow rate of 0.3 mL/min using a piece of 60-cm length Supelco-Q plot capillary column as the extraction capillary. The quantitative study was explored by operating in selected-ion monitoring (SIM) mode. The calibration curves were linear in the range from 0.5 ng/mL or 2 ng/mL to 500 ng/mL. The detection limits were from 0.02 ng/mL to 2 ng/mL. At the optimized capillary and fragmentor voltages, the characteristic ions for each compound clearly showed up in the spectra and it is possible to use the LC-MS to identify these compounds. The method was applied to the analysis of biological samples without interfering peaks. However, the recoveries for some of the compounds in serum samples need to be further improved.