刑事技术Issue(1)：46-49,4.DOI:10.16467/j.1008-3650.2016.01.009
超高效液相色谱-质谱定量测定全血中的13种苯二氮卓类安眠镇静药物
Simultaneous Quantiifcation of Thirteen Benzodiazepines and Metabolites in Whole Blood by UPLC-MS/MS
王朝虹 1张琳 1赵蒙 1刘勇 1褚建新 2蒋文慧3
作者信息
- 1. 最高人民检察院检察技术信息研究中心，北京 100040
- 2. 浙江省检察院，杭州 310012
- 3. 杭州市检察院，杭州 310000
- 折叠
摘要
Abstract
ABSTRACT:A rapid and sensitive method has been developed for simultaneous determination of 13 benzodiazepines and metabolites including diazepam, nitrazepam, bromazepam, lfurazepam, clonazepam, lfunitrazepam, lorazepam, oxazepam, prazepam, temazepam, 7-amino-nitragepam, 7-aminoflunitrazepam and chlordiazepam in whole blood samples by ultra-performance liquid chromatography coupled with mass spectrometry (UPLC-MS/MS). The separations were carried out on an ACQULTY UPLC BEH C18 column (2.1 mm ×100 mm, 1.7 μm) at 35°C and with a constant lfow rate of 0.5 mL/min and the gradient-elution consisting of acetonitrile and 5 mmoL ammonium hydrogen carbonate buffer. The MS parameters were set as capillary voltage (3 kV), desolvation gas temperature (550°C), desolvation gas lfow (800 L/h), cone gas lfow (150 L/h) and collision gas lfow (0.15 mL/min). OstraTM 96-well plate was used to extract the samples. 100 μL of human whole blood containing target drugs and D5-diazepam as internal standard was transferred into the OstraTM 96-well plate, followed by 400 μL of 0.1% formic acid in acetonitrile. Phospholipids were removed from the whole blood via the OstraTM 96-well plate effectively, and the ifltrate was collected under a constant pressure of 20 psi. Thereafter, the 96-well receiving plate was capped and placed on the suitable position in sample manager and was analyzed with UPLC-MS/MS system coupled with an electrospray ionization (ESI) source. The samples were measured in the mode of electraspray positive ionization (ESI+) and multiple reaction monitoring (MRM). 13 benzodiazepines and metabolites were linear in the range of 0.2~20 ng/mL with coefifcients higher than 0.99. The extraction recoveries ranged from 65.2% to 113.9% for all analytes, and the limits of detection (LODs) were 0.008~0.15 ng/mL. The method presented here is validated to be simple, rapid, sensitive and accurate for the determination of trace benzodiazepines and metabolites in whole blood samples.关键词
苯二氮卓类药物/超高效液相色谱-串联四级杆质谱/全血/ostro磷脂过滤板Key words
benzodiazepines/UPLC-MS/MS/whole blood/OstraTM 96-well plate分类
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王朝虹,张琳,赵蒙,刘勇,褚建新,蒋文慧..超高效液相色谱-质谱定量测定全血中的13种苯二氮卓类安眠镇静药物[J].刑事技术,2016,(1):46-49,4.
