超高效液相色谱-三重四极杆质谱法检测血中脱乙基扎来普隆
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摘要
建立了全血中脱乙基扎来普隆液相色谱-串联质谱检验法。对p H、淋洗液、缓冲液等条件进行优化,实验选用HLB柱,p H 9硼酸盐缓冲溶液,氨水-甲醇水为淋洗液,乙腈为洗脱液,选用ZORBAX Eclipse Plus C18色谱柱,以A相0.1%甲酸和B相乙腈作为流动相,进行梯度洗脱。采用液相色谱-串联质谱仪的电喷雾电离,正离子模式扫描,MRM模式检测脱乙基扎来普隆。在最优条件下,全血中脱乙基扎来普隆质量浓度在0.1~100 ng/m L范围内有良好线性关系,保留时间为1.95 min。回归方程为y=9971.2ρ-1 813.8,检出限0.1 ng/m L。回收率90%以上,日内与日间精密度均小于10%。方法适用于全血中的脱乙基扎来普隆检测。
We established a liquid chromatography tandem mass spectrometry( UPLC / MS / MS) assay for the determination of zaleplon main metabolite desethylzaleplon in plasma samples. The target drugs were extracted from plasma and then detected with liquid chromatography tandem mass spectrometry( UPLC / MS / MS). The SPE purification was performed with Oasis HLB 3m L cartridges previously conditioned with methanol and equilibrated with buffer solution. The mixtures of sample and buffer were loaded on the cartridge and slowly passed through the bed without vacuum. Then the cartridges column was rinsed sequentially with buffer solution and ammonia in methanol-water. After drying the column,the retained drugs were eluted with acetonitrile. The mobile phases consisted of acetonitrile( mobile phase B) and water containing 0. 1% formic acid( mobile phase A). MS-MS in the multiple reaction monitoring( MRM) mode was performed in positive electrospray ionization( ESI+). The retention time of desethylzaleplon was 1. 95 min. The linear relationship was excellent between0. 1 ~ 100 ng / m L. Regression equation was y = 9 971. 2ρ-1 813. 8 and the limit of detection for desethylzaleplon was 0. 1 ng / m L. The recovery of desethylzaleplon was more than 90%. The inter-day and intraday precisions were less than 10%. This rapid, accurate and sensitive method can be used in forensic toxicological analysis.
We established a liquid chromatography tandem mass spectrometry( UPLC / MS / MS) assay for the determination of zaleplon main metabolite desethylzaleplon in plasma samples. The target drugs were extracted from plasma and then detected with liquid chromatography tandem mass spectrometry( UPLC / MS / MS). The SPE purification was performed with Oasis HLB 3m L cartridges previously conditioned with methanol and equilibrated with buffer solution. The mixtures of sample and buffer were loaded on the cartridge and slowly passed through the bed without vacuum. Then the cartridges column was rinsed sequentially with buffer solution and ammonia in methanol-water. After drying the column,the retained drugs were eluted with acetonitrile. The mobile phases consisted of acetonitrile( mobile phase B) and water containing 0. 1% formic acid( mobile phase A). MS-MS in the multiple reaction monitoring( MRM) mode was performed in positive electrospray ionization( ESI+). The retention time of desethylzaleplon was 1. 95 min. The linear relationship was excellent between0. 1 ~ 100 ng / m L. Regression equation was y = 9 971. 2ρ-1 813. 8 and the limit of detection for desethylzaleplon was 0. 1 ng / m L. The recovery of desethylzaleplon was more than 90%. The inter-day and intraday precisions were less than 10%. This rapid, accurate and sensitive method can be used in forensic toxicological analysis.
引文
[1]郭璟琦,石银涛,王侩军.分析试验室,2014,33(9):1055
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[3]马仁玲,周红华,刘文华,等.中国药科大学学报,2003,34(4):330
[4]邓鸣,张素芬,刘建芳.药物分析杂志,2004,24(6):611
[5]吴海,晏晓军,高汨,等.刑事技术,2013,(2):22
[6]Luca Anzillotti,Sara Odoardi,Sabina Strano-Rossi.Forensic Sci Int,2014,243:99
[7]张蕾萍,于忠山,何毅,等.刑事技术,2011,(1):13
[2]张蕾萍,黄霜,舒翠霞.刑事技术,2015,40(1):122
[3]马仁玲,周红华,刘文华,等.中国药科大学学报,2003,34(4):330
[4]邓鸣,张素芬,刘建芳.药物分析杂志,2004,24(6):611
[5]吴海,晏晓军,高汨,等.刑事技术,2013,(2):22
[6]Luca Anzillotti,Sara Odoardi,Sabina Strano-Rossi.Forensic Sci Int,2014,243:99
[7]张蕾萍,于忠山,何毅,等.刑事技术,2011,(1):13