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目的建立食品中高氯酸盐的超高效液相色谱-串联质谱(UPLC-MS/MS)的测定方法。方法香辛料调味品用水提取,蔬菜、水果用乙腈-水(1∶1,V/V)提取,肉、禽、蛋、奶和水产品用乙腈-水(2∶1,V/V)提取,C_(18)柱(3 ml,200 mg)净化,以高氯酸根为内标定量,采用UPLC-MS/MS法测定。结果在0.3~20.0μg/L范围内,3种提取溶液中高氯酸盐有良好的线性关系,R~2≥0.999。加标浓度在2.0~50.0μg/kg范围内,内标相对平均回收率为82.6%~108.6%,相对标准偏差(RSD)为1.0%~9.9%。牛奶的定量限为2.0μg/kg,其他食品的定量限为10.0μg/kg。结论本方法简单快捷,定量准确,适用于食品中高氯酸盐的测定。
Objective To establish a method for the determination of perchlorate in food by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS / MS). Methods Spices and condiments were extracted with water and fruits and vegetables were extracted with acetonitrile-water (1: 1, V / V) The C_ (18) column (3 ml, 200 mg) was purified and the content of perchlorate as internal standard was determined by UPLC-MS / MS. Results In the range of 0.3 ~ 20.0μg / L, there was a good linear relationship between perchlorate in the three extraction solutions, R ~ 2≥0.999. The relative standard deviations (RSDs) ranged from 1.0% to 9.9%, with the average recoveries of 82.6% -108.6% and the relative standard deviations (RSDs) within the range of 2.0-50.0 μg / kg. The limit of quantitation of milk is 2.0μg / kg, and the limit of quantitation of other foods is 10.0μg / kg. Conclusion The method is simple, rapid and accurate. It is suitable for the determination of perchlorate in food.