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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。
Established in the whole blood de-ethyl Zaleplon liquid chromatography-tandem mass spectrometry. The conditions of p H, eluent and buffer were optimized. HLB column, p H 9 borate buffer solution, ammonia-methanol water as eluent and acetonitrile as eluent were selected for experiment. ZORBAX Eclipse Plus C18 Column, with phase A 0.1% formic acid and B phase acetonitrile as the mobile phase, gradient elution. Electrospray ionization, positive ion mode scanning and tandem mass spectrometry (MRM) were used to detect the deprotection of zaleplon. Under optimal conditions, the concentration of ethyl-zaleplon in whole blood had a good linearity within the range of 0.1-100 ng / mL, with a retention time of 1.95 min. The regression equation was y = 9971.2ρ-1 813.8 with a detection limit of 0.1 ng / m L. The recovery rate is more than 90%, with the precision of less than 10% on day and day. The method is suitable for the deprotection of zaleplon in whole blood.