高效液相色谱-串联质谱法测定牛奶中的高氯酸盐和氯酸盐

摘要

A method for the simultaneous determination of perchlorate and chlorate in milk was developed using high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS).Acetonitrile-methanol-acetic acid (90∶ 10∶ 1,v/v/v) was chosen to extract the target analytes and to precipitate the protein in milk sample,followed by a cleanup procedure with hexane for removing the fat.The analytes were separated in non-modified porous graphitic carbon column (Hypercarb).A triple quadrupole mass spectrometry equipped with an electrospray ionization source was used to detect the perchlorate and chlorate.The good correlation coefficients (r2＞0.999) are obtained within their respective linear ranges.The limits of quantification (S/N=10) of perchlorate and chlorate are 0.8 μg/kg and 3 μg/kg respectively.The mean recoveries of two compounds are from 83.8％ to 97.3％ with RSDs from 2.2％ to 8.8％.%建立了高效液相色谱-串联质谱(HPLC-MS/MS)同时检测牛奶中高氯酸盐和氯酸盐的分析方法.样品用乙腈-甲醇-乙酸溶液(90∶10∶1,体积比)提取同时沉淀蛋白,正己烷去除脂肪,在非修饰多孔石墨化碳柱(Hypercarb)上进行分离,然后采用电喷雾离子化三重四极杆串联质谱测定.结果表明,高氯酸盐和氯酸盐在各自的线性范围内峰面积与其质量浓度线性关系良好,相关系数(r2)大于0.999;高氯酸盐的定量限(S/N=10)为0.8 μg/kg,氯酸盐的定量限为3μg/kg;两种化合物的平均回收率为83.8％～97.3％,相对标准偏差为2.2％ ～ 8.8％.