超高效液相色谱-串联质谱法同时测定食品中的氯酸盐和高氯酸盐残留量

Simultaneous determination of chlorate and perchlorate in foods by ultra performance liquid chromatography-tandem mass spectrometry

目的建立超高效液相色谱-串联质谱法测定食品中氯酸盐和高氯酸盐残留量的方法。方法食品样品经纯水溶解,乙腈提取,固相萃取柱净化,排除复杂基体干扰,超高效液相色谱-串联质谱仪测定。采用多反应监测模式,电喷雾电离源负离子模式,内标法定量。结果氯酸盐在0.5~200ng/mL、高氯酸盐在0.1~100ng/mL范围内线性关系良好,相关系数(r2)均大于0.99,检出限(S/N=3)为氯酸盐6.0μg/kg和高氯酸盐1.0μg/kg,定量限(S/N≥10)为氯酸盐18.0μg/kg和高氯酸盐3.0μg/kg。以不含氯酸盐和高氯酸盐的样品作为空白样品进行添加回收实验,氯酸盐的回收率为83.7%~108.7%,相对标准偏差为1.7%~6.2%,高氯酸盐的回收率为87.8%~112.8%,相对标准偏差为1.9%~7.5%。结论该方法不但可以有效排除复杂基体的干扰,而且简单、灵敏、稳定,适用于多种食品复杂基体中的氯酸盐和高氯酸盐残留量的测定。

Objective To establish a method for simultaneous determination of chlorate and perchlorate residues in foods by ultra performance liquid chromatography-tandem mass spectrometry. Methods The food samples were dissolved in pure water, extracted with acetonitrile, purified by solid phase extraction column to eliminate the interference of complex matrix, then determined by ultra performance liquid chromatography-tandem mass spectrometer with multi-reaction monitoring mode and negative ion mode of electrospray ionization source, and quantified by internal standard method. Results The calibration curves showed a good linearity in the range of 0.5-200 ng/mL for chlorate and 0.1-100 ng/mL for perchlorate with r2≥0.99. The limits of detection of chlorate and perchlorate(S/N=3) were 6.0 μg/kg and 1.0 μg/kg, and the limits of quantitation of chlorate and perchlorate(S/N≥10) were 18.0 μg/kg and 3.0 μg/kg. The samples without chlorate and perchlorate were used as blank samples for addition and recovery test, the recoveries of chlorate were 83.7%-108.7%, and the relative standard deviations were1.7%-6.2%, the recoveries of perchlorate were 87.8%-112.8%, and the relative standard deviations were 1.9%-7.5%. Conclusion This method not only can effectively eliminate the interference of complex matrix, but also is simple, sensitive and stable, which is suitable for the determination of chlorate and perchlorate residues in a variety of food complex matrices.