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建立高效液相-串联质谱法测定青刀豆中的毒死蜱代谢物磷酸二乙酯残留量的检测方法。青刀豆样品经盐酸酸化后用乙腈提取,提取液经活性炭固相萃取小柱净化,以Thermo Scientific Waters SpherisorbRR column-NH2色谱柱为分析柱,乙酸铵水溶液和乙腈体系为流动相,等梯度淋洗。检测器采用三重四极杆串联质谱仪,配备电喷雾电离源,在负离子扫描模式下采用选择反应监测,定量离子为m/z153>125,定性离子为m/z153>125,79。该方法检测磷酸二乙酯在16μg·L-1到8000μg·L-1范围内有良好的线性关系,方法定量限(S/N=10)为2μg·kg-1,加标回收率为83%～90%,测定值的相对标准偏差小于9.8%。
To establish a high performance liquid chromatography-tandem mass spectrometry (HPLC-MS / MS) method for the determination of diethylphosphate metabolites in chlorpyrifos. The samples of green beans were acidified with hydrochloric acid and extracted with acetonitrile. The extracts were purified by solid-phase extraction on activated carbon cartridges. The column was on a Thermo Scientific Waters SpherisorbRR column-NH2 column. The aqueous ammonium acetate solution and acetonitrile were mobile phase, wash. The detector uses a triple quadrupole tandem mass spectrometer equipped with an electrospray ionization source and is monitored by selective reaction in anionscan mode with m / z153> 125 for the quantified ions and m / z153> 125,79 for the qualifier ions. The method has good linearity in the range of 16μg · L-1 to 8000μg · L-1. The limit of quantification (S / N = 10) was 2μg · kg-1 and the recovery was 83 % ~ 90%, the relative standard deviation of the measured value is less than 9.8%.