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 The perchlorate residue in spices and condiments was extracted with water,that in vegetables and fruits was extracted with acetonitrile-water( 1∶ 1,V/V),and that in meat,poultry,eggs,milk and aquatic products was extracted with acetonitrile-water( 2 ∶ 1,V/V). The supernatant was cleaned up with C(18)SPE( 3 ml,200 mg),and the detection was carried out by UPLC-MS/MS with internal standardmethod for quantification. Results The calibration curve was linear in the concentration range of 0. 3-20. 0 μg/L( R^2≥0. 999),the recovery was in the range of 82. 6%-108. 6%,the relative standard deviation( RSD) was in the range of 1. 0%-9. 9%,and the limit of detection was 2. 0 μg/kg for milk,and 10. 0 μg/kg for other food. Conclusion The method was simple,accurate and highly sensitive,and suitable for the determination of perchlorate in food.