血清中16种有机磷农药GC/MS/MS检测方法的研究

Determination of 16 kinds of organophosphorus pesticides in serum by using GC/MS/MS

目的应用GC/MS/MS建立测定血清中敌敌畏、氧化乐果等16种有机磷农药的分析方法。方法首先做GC/MS全扫描分析,确定16种化合物的母离子,然后比较不同碰撞诱导裂解(CID)电压时二级质谱中特征离子的峰面积大小以及信噪比,对CID电压进行优化,从而确定各化合物的色谱质谱条件。样品用Oasis HLB小柱进行固相萃取后,用乙酸乙酯洗脱,浓缩后再用乙酸乙酯定容后上机测定。结果在0～1000ng/ml范围内,16种化合物的线性相关系数均大于0.995,加标回收率在75%～129%之间,RSD<10%;日内和日间相对标准偏差小于15%(n=6)。除敌敌畏的检测限为55ng/ml外,其余待测物均检出限均小于2ng/ml。结论该方法灵敏度高、准确性好,适合于血清中有机磷农药的分析测定。

Objective To establish a method of determining the presence and concentration of 16 kinds of organopbosphorus pesticides in serum by GC/MS/MS. Method The parent ions of each pesticide was detected by running GC/MS in a full scan mode, and the peak areas and the ratio of signal to noise of each product ion were compared by setting different CID voltages. The CID voltage for each parent ion was optimized and determined. Serum samples were solid-phase extracted by Oasis HLB and eluted with ethyl ether after being concentrated and made to constant volume with ethyl ether, and then were tested by GC/MS/MS. Results The correlation coefficient for each compound in the range of 0 - 1000ng/ml was greater than 0. 990. Recoveries of standard addition were 75% - 129% ,RSD 〈 10%. The intra-day and inter-day RSD was less than 15% （n = 6）. The limits of quantification were less than 2ng/ml except for dichlorovos （55ng/ml）. Conclusion GC/MS/MS assay is sensitive and accurate for the determination of pesticides in serum.