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本研究建立了超高效液相色谱-串联质谱法测定人血浆中的7种影响驾驶安全的药物——赛庚啶、西替利嗪、氯苯那敏、艾司唑仑、劳拉西泮、氯硝西泮和地西泮,这些药物是中药制剂和保健品中易违禁添加的化学成分。以奥沙西泮为内标,使用Acquity UPLC HSS C_(18)色谱柱,流动相为0.01%甲酸水溶液∶0.01%甲酸甲醇溶液,线性梯度洗脱。质谱采用电喷雾离子源,多反应监测模式,正离子分段扫描分析。结果表明,赛庚啶、西替利嗪、氯苯那敏、艾司唑仑、劳拉西泮、氯硝西泮和地西泮分别在3.75~3.00×10~3、2.00~2.00×10~3、0.25~1.00×10~2、2.04~2.04×10~3、2.08~2.08×10~3、2.08~2.08×10~3和2.65~1.06×10~3 ng/ml范围内线性关系良好;最低检测限(LLOD)分别为0.38、0.50、0.10、0.51、0.52、0.52和0.05 ng/ml。日内、日间RSD均小于15%;提取回收率均大于70%,RSD<15%。内标的提取率为(80.67±4.29)%(RSD=5.32%)。该方法操作简便、灵敏度高、专属性强,可用于上述7种化合物血药浓度的测定。
In this study, ultra high performance liquid chromatography-tandem mass spectrometry (HPLC-MS / MS) was developed for the determination of seven kinds of drugs that affect driving safety in human plasma-cyproheptadine, cetirizine, chlorpheniramine, estazolam, lorazepam , Clonazepam and diazepam, these chemicals are easily added to the chemical composition of traditional Chinese medicine preparations and health products. Using oxazepam as the internal standard, the mobile phase was eluted with a linearity gradient of 0.01% formic acid in methanol and 0.01% formic acid on an Acquity UPLC HSC C 18 column. Mass spectrometry using electrospray ionization, multi-reaction monitoring mode, positive ion segmentation scanning analysis. The results showed that cyproheptadine, cetirizine, chlorpheniramine, estazolam, lorazepam, clonazepam and diazepam were 3.75 ~ 3.00 × 10 ~ 3,2.00 ~ 2.00 × 10 ~ 3,0.25 ~ 1.00 × 10 ~ 2,2.04 ~ 2.04 × 10 ~ 3,2.08 ~ 2.08 × 10 ~ 3,2.08 ~ 2.08 × 10 ~ 3 and 2.65 ~ 1.06 × 10 ~ 3 ng / ml ; Minimum detectable limit (LLOD) were 0.38,0.50,0.10,0.51,0.52,0.52 and 0.05 ng / ml. The intra-day and inter-day RSD were less than 15%. The recovery rates were both above 70% and RSD <15%. The internal standard extraction rate was (80.67 ± 4.29)% (RSD = 5.32%). The method is simple, high sensitivity and specificity, and can be used for the determination of blood concentration of the above seven compounds.