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目的建立在线凝胶渗透色谱—气相色谱质谱法测定粮食中毒死蜱的残留量。方法以毒死蜱-D10为内标,参照QuEChERS的样品前处理方法,用乙腈进行提取,采用分散固相萃取技术净化,在线凝胶渗透色谱—气相色谱质谱法进行检测,凝胶渗透色谱系统使用Shodex CLNpak EV-200凝胶色谱柱,柱箱温度设为40℃,流动相为丙酮/环己烷(3/7,v/v),流速为0.1 ml/min,进样量为10μl;气相色谱质谱系统采用氦气为载气,进样口和柱箱采用程序升温方式,Rxi-5ms毛细管色谱柱分离,采用Scan/SIM同时测定的方法,根据保留时间和特征离子进行定性,内标法定量。结果毒死蜱在0.005 mg/L~0.25 mg/L范围内有好的线性(r=0.9998),方法检出限为0.003 mg/kg,样品的加标回收率为97.8%~104.8%,RSD<5.0%。结论所建立的方法简便、快速、准确,可用于粮食中毒死蜱残留量的检测。
OBJECTIVE To establish an online gel permeation chromatography-gas chromatography-mass spectrometry method for the determination of chlorpyrifos residue in food. Methods Chlorpyrifos-D10 was used as an internal standard. According to the QuEChERS sample pretreatment method, acetonitrile was used for extraction. The samples were purified by dispersive solid-phase extraction (SPE-GC) and detected by on-line gel permeation chromatography-gas chromatography mass spectrometry. The gel permeation chromatography system was Shodex CLNpak EV-200 gel column with an oven temperature of 40 ° C and a mobile phase of acetone / cyclohexane (3/7, v / v) at a flow rate of 0.1 ml / min with an injection volume of 10 μl; gas chromatography Mass spectrometry system using helium as carrier gas, inlet and oven temperature programmed, Rxi-5ms capillary column separation, using the simultaneous determination of Scan / SIM method, according to retention time and characterization of ions qualitative, internal standard method of quantification . Results The chlorpyrifos showed a good linearity (r = 0.9998) in the range of 0.005 mg / L ~ 0.25 mg / L with the detection limit of 0.003 mg / kg and the spiked recoveries of 97.8% ~ 104.8% %. Conclusion The established method is simple, rapid and accurate and can be used for the determination of chlorpyrifos in food.