摘要
目的建立唾液中奥沙西泮的超高液相色谱—串联质谱(UPLC-MS/MS)检测方法。方法液相色谱仪采用流动相为乙腈-0.1%甲酸水溶液进行梯度方式洗脱。串联质谱仪采用电喷雾离子源正离子(ESI+)多反应监测(MRM)模式进行质谱分析,用287.0/241.0、287.0/165.0和287.0/104.0这3对特征离子对和保留时间对奥沙西泮进行定性分析,采用外标标准曲线法对奥沙西泮进行定量分析。唾液样品经甲醇稀释后,经振荡器振荡3 min,在15 000 r·min^(-1)转速下离心3 min,取上清液过有机滤膜(13 mm×0.22μm)后待检。结果奥沙西泮在1~100 ng·mL^(-1)线性范围内,线性方程:A=3 700×C+2 390,线性关系良好(R2=0.9 999),检出限和定量限分别为0.09 ng·mL^(-1)和0.30 ng·mL^(-1);奥沙西泮的提取回收率均高于90%,日内及日间精密度小于10%。结论本方法简便、快速、定量准确,适用于检测唾液中的奥沙西泮。
Objective A method of determination of oxazepam in saliva was established by UPLC-MS/MS method. Methods The ultra high performance liquid chromatograph was using the mobile phase contisted of ACN（ eluent A） and 0. 1% FA in water（ eluent B） which was running in gradient elution way.The mass spectrometric acquisition was carried out by electospray ionization in positive mode（ ESI＋） with multiple reaction monitoring（ MRM） method,multiple characteristic ion pairs（ 287. 0/241. 0,287. 0/165. 0 and 287. 0/104. 0） and retention time were adopted to oxazepam for qualitative analysis,and the external standard method was adopted to oxazepam for quantitative analysis. The samples were diluted with methanol reagent,and the samples diluted were oscillated for 3 min,centrifuged for 3 min at 15 000 r · min^-1,the supernatant liquor was to be detected after purificated by organic membrane filter. Results The linear ranges were 1 - 100 ng · mL^-1 for oxazepam,the linear equation： A = 3 700 × C ＋ 2 390,and the linear relationship was good with the correlation coefficient was 0. 9 999,the qualitative and quantitative restriction were 0. 09 ng·mL^-1 and 0. 30 ng·mL^-1 respectively in the saliva. The extract recovery of oxazepam was above 90%,intra-and inter-day precisions were all less than 10%. Conclusion This method is simple、rapid and accurate for determination of oxazepam in saliva.
作者
吴东星
李树华
李继印
任国印
曾思火
李虹
WU Dong-xing1, LI Shu-hua2, LI Ji-yin3 , REN Guo-yin3, ZENG Si-huo3, LI Hong3(1. Institute of Forensic, Kunming Medical University, Kunming 650500, China; 2. Key Laboratory of Narcotics Assay and Control Technology, Ministry of Public Security, Kunming 650228, Chin)
出处
《河南科技大学学报（医学版）》
2018年第2期137-140,共4页
Journal of Henan University of Science & Technology:Medical Science
作者简介
吴东星（1990-），男，土家族，湖北利川人，从事法医药、毒物分析研究。;通信作者：李虹，女，主任法医师，E—mail：yngalh@163．com
