超高效液相色谱-串联质谱法测定血液中20种常见毒品

UHPLC-MS/MS Determination of 20 Common Drugs in Blood

血液样品用乙腈提取,再以8 000r·min^-1转速离心10min,取上清液,经0.22μm有机滤膜过滤,采用超高效液相色谱-串联质谱法测定滤液中20种常见毒品的含量。以ACQUITY UPLC HSS C18色谱柱为固定相,以不同体积比的乙腈和pH 3.0的5mmol·L^-1甲酸铵溶液的混合液为流动相进行梯度洗脱,串联质谱分析中采用电喷雾正离子源和多反应监测模式。20种毒品的质量浓度均在10.0~100μg·L^-1内与其对应的峰面积呈线性关系,检出限(3S/N)为0.10~5.00μg·L^-1。以空白样品为基体进行加标回收试验,所得回收率为42.3%~113%,测定值的日内相对标准偏差(n=5)为0.050%~15%,日间相对标准偏差(n=3)为2.1%~15%。

The blood sample was extracted with acetonitrile,and then centrifugated for 10 min at the speed of8 000 r· min^-1.The supernatant was filtered on 0.22μm organic filtration membrane.UHPLC-MS/MS was applied to the determination of 20 common drugs in the filtrate.ACQUITY UPLC HSS C18 chromatographic column was used as stationary phase,and the mixture of acetonitrile and 5 mmol·L^-1 ammonium formate solution(pH3.0)mixed in different ratios was used as mobile phase in gradient elution.ESI+and multi-reactions monitor mode were adopted in MS/MS.Linear relationships between values of peak area and mass concentration of the 20 drugs were kept in the same range of 10.0-100μg·L^-1,with detection limits(3 S/N)in the range of 0.10-5.00μg·L^-1.On the base of blank sample,test for recovery was made by standard addition method;values of recovery found were in the range of 42.3%-113%,with intra-day RSDs(n=5)and inter-day RSDs(n=3)of determined values in the ranges of 0.050%-15% and 2.1%-15%,respectively.