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超高效液相色谱-串联质谱法测定婴幼儿配方奶粉中氯酸盐和高氯酸盐 被引量:11

Determination of chlorate and perchlorate in infant formula by ultra-high performance liquid chromatography-tandem mass spectrometry
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摘要 目的建立超高效液相色谱-串联质谱法(ultra-high performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)同时测定婴幼儿配方奶粉中氯酸盐和高氯酸盐的分析方法。方法氯酸盐-18O3和高氯酸盐-18O4加入到样品中,通过涡旋混合、提取、离心和过滤,收集滤液,待UPLC-MS/MS分析。流动相为20 mmol/L甲酸铵和乙腈。Waters TorusTM DEA(2.1 mm×100 mm, 1.7μm)色谱柱用来分析高氯酸盐和氯酸盐。采用负电喷雾电离,多反应监测模式,内标法定量。结果氯酸盐和高氯酸盐分别在0.2~200μg/L和0.1~100μg/L范围内线性关系良好(R2>0.999),方法检出限分别为0.35和0.12μg/kg,定量限分别为1.16和0.40μg/kg。在15.0、75.0和150μg/kg加标水平下,氯酸盐回收率为91.9%~102.8%,相对标准偏差为2.5%~4.4%(n=6)。在7.5、37.5和75.0μg/kg加标水平下,高氯酸盐的回收率为91.3%~106.3%,相对标准偏差为2.6%~3.9%(n=6)。结论该方法简便、快速、灵敏度高、准确性好,适用于各类复杂基质中高氯酸盐和氯酸盐的同时分析。 OBJECTIVE To establish a method for determination of perchlorate and chlorate in infant formula by ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS). METHODS Chlorate-18O3 and perchlorate-18O4 were added to the samples, and the filtrate was collected and analyzed by UPLC-MS/MS by vortex mixing, extraction, centrifugation and filtration. The mobile phase was 20 mmol/L ammonium formate and acetonitrile. The Waters TorusTM DEA(2.1 mm×100 mm, 1.7 μm)column was used to separate chlorate and perchlorate. The negative spray ionization(ESI-) was used. The multi-response monitoring(MRM) mode was used for monitoring. The internal standard method was used for quantification. RESULTS The linear relationships of chlorate and perchlorate were good in the range of 0.2-200 μg/L and 0.1-100 μg/L(R2>0.999), respectively. The detection limits(LOD, S/N=3) of chlorate and perchlorate were 0.35 μg/kg and 0.12 μg/kg, respectively, and the quantitative limits(LOQ, S/N=10) of chlorate and perchlorate were 1.16 μg/kg and 0.40 μg/kg, respectively. At the addition levels of 15.0, 75.0 and 150 μg/kg, the chlorate recovery was 91.9%-102.8% and the relative standard deviation(RSD, n=6) was 2.5%-4.4%.At the addition levels of 7.5, 37.5 and 75.0 μg/kg, the recovery rate of perchlorate was 91.3%-106.3% and the RSD(n=6) was 2.6%-3.9%. CONCLUSTION The method is simple, rapid, sensitive and accurate, and is suitable for simultaneous analysis of perchlorate and chlorate in various complex substrates.
作者 张文婷 华永有 陆秋艳 邱文倩 李宇翔 Zhang Wenting;Hua Yongyou;Lu Qiuyan;Qiu Wenqian;Li Yuxiang(Fujian Provincial Key Laboratory of Zoonosis Research,Fujian Center for Disease Control&Prevention,Fuzhou 350001,China)
出处 《卫生研究》 CAS CSCD 北大核心 2021年第4期625-632,共8页 Journal of Hygiene Research
基金 福建省卫生健康委青年课题(No.2016-2-10)。
关键词 婴幼儿配方奶粉 氯酸盐 高氯酸盐 超高效液相色谱-串联质谱 infant formula chlorate perchlorate ultra-high performance liquid chromatography-tandem mass spectrometry
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