高效液相色谱-串联质谱法测定生物样品中4,4′-二氨基-3,3′-二氯二苯甲烷残留

Determination of 4,4′-Methylene Bis-(2-chloroaniline)Residue in Biological Samples by High Performance Liquid Chromatography-Tandem Mass Spectrometry

通过优化样品前处理方法、色谱及质谱条件,建立了血液和尿液2种生物样品中高关注度化学品4,4′-二氨基-3,3′-二氯二苯甲烷（MOCA）的高效液相色谱-串联质谱检测方法。样品采用不同比例乙腈提取,经C18柱净化,以乙腈-0.1%HAc溶液作流动相,等度洗脱,经Agilent Eclipse AAA色谱柱分离后,质谱检测。分别以267.3〉231.0为定量离子对,267.3〉195.2、267.3〉140.0为定性离子对进行MOCA的定性定量分析。方法线性范围为：血液1.0~100.0ng/mL（相关系数为0.9998）,尿液0.5~50.0ng/mL（相关系数为0.9999）;回收率范围为：血液81.0%~89.7%（相对标准偏差为5.76%~8.47%）,尿液84.0%~95.0%（相对标准偏差为2.87%~7.54%）。该方法灵敏度高、重复性好、操作简便,可用于高危人群MOCA的健康风险监测。

A high performance liquid chromatography-tandem mass spectrometric（HPLC-MS/MS）method was developed for the determination of 4,4′-methylene bis-（2-chloroaniline）（MOCA）in blood and urine samples.Samples were extracted by acetonitrile,purified by C18 column,separated with Agilent Eclipse AAA column using acetonitrile and 0.1% acetic acid as mobile phase,and determined by 267.3〉231.0;267.3〉195.2and 267.3〉140.0ion pairs.Results showed that the linearity of blood sample ranged from 1.0-100.0ng/mL with the correlation coefficient of 0.9998,the linearity of urine sample ranged from 0.5-50.0ng/mL with the correlation coefficient of 0.9999.The recoveries of blood sample ranged from81.0%to 89.7% with the relative standard deviation of 5.76%-8.47%,and the recoveries of urine sample ranged from 84.0% to 95.0% with the relative standard deviation of 2.87%-7.54%.The proposed method was successfully applied to the determination of the compounds in related samples,which provides a simple,convenient means for health risk monitoring among high-risk groups of MOCA.