Direct and LC analysis of five benzodiazepines in human urine plasma using an ADS restricted access extraction column
Direct and LC analysis of five benzodiazepines in human urine plasma using an ADS restricted access extraction column
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DOI：
10.1016/s0731-7085(01)00461-7
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发表时间：
2001-12-01
影响因子：
3.4
通讯作者：
Pawliszyn, J
中科院分区：
文献类型：
--
作者：
Mullett, WM;Pawliszyn, J
采用烷基二醇硅胶（ADS）预柱直接在线萃取血清和尿液中的几种苯二氮卓类药物。将生物样品中的蛋白质组分通过ADS柱，同时萃取ADS固定相孔中的苯二氮卓类化合物，证实了疏水作用在萃取机理中的作用。采用柱切换技术将ADS柱中提取的待测物固定到高效液相色谱反相C18柱中，进行苯二氮卓类药物的等度分离和紫外检测。通过大体积进样的样品预浓缩是可能的，提高了检测限。血清中氯硝西泮、奥沙西泮、替马西泮、去甲西泮和地西泮的检出限分别为38.8、24.2、31.7、31.3和45.0 ng/ml;尿液中氯硝西泮、奥沙西泮、替马西泮、去甲西泮和地西泮的检出限分别为48.4、24.5、31.7、33.1和52.9 ng/ml。在两种基质中，该方法在50-10000 ng/ml范围内呈线性，平均线性系数（R-2）值为0.9918。在10次进样中评价了该方法的进样重复性和测定内精密度，结果相对标准偏差<5%。ADS萃取柱具有耐用性，可直接进样多种生物液体，用于苯二氮卓类药物的萃取和后续测定。(C)2001 Elsevier Science B. V.保留所有权利。
An alkyl-diol-silica (ADS) precolumn was used for the direct and on-line extraction of several benzodiazepines from serum and urine. The protein component of the biological sample was flushed through the ADS column, while simultaneously extracting the benzodiazepine compounds in the pores of the ADS stationary phase, The role of hydrophobic interactions in the extraction mechanism was confirmed. Column switching was employed to elute the extracted analytes from the ADS column into a high-performance liquid chromatography reverse-phase C18 column for the isocratic separation and UV detection of the benzodiazepines. Sample preconcentration via large volume injections was possible, improving the limits of detection. The calculated clonazepam, oxazepam, temazepam, nordazepam and diazepam detection limits were 38.8, 24.2, 31.7, 31.3, 45.0 ng/ml in serum, respectively, and 48.4, 24.5, 31.7, 33.1, 52.9 ng/ml for urine, respectively. The method was linear over the range of 50-10000 ng/ml in both matrices with an average linear coefficient (R-2) value of 0.9918. The injection repeatability and intra-assay precision of the method were evaluated over ten injections, resulting in a percent relative standard deviation < 5%. The ADS extraction column was robust, providing many direct injections of biological fluids for the extraction and subsequent determination of benzodiazepines. (C) 2001 Elsevier Science B.V. All rights reserved.