超高效液相色谱-串联质谱法测定饮料中高氯酸盐和氯酸盐
Determination of perchlorate and chlorate in drinks by ultra-performance liquid chromatography-tandem mass spectrometry
陈东 1李倩 2刘平 1陈忠辉 1谢昀 3许秀丽 3张晶 1张峰3
作者信息
- 1. 北京市疾病预防控制中心,食物中毒诊断溯源技术北京市重点实验室,北京 100013
- 2. 北京市大兴区疾病预防控制中心,北京 102600
- 3. 中国检验检疫科学研究院,北京 100176
- 折叠
摘要
目的 建立同位素内标法定量测定饮料中高氯酸盐和氯酸盐的高效液相色谱-串联质谱法.方法 液体饮料样品经甲醇溶液提取,固体饮料样品经乙酸水提取,PSA/C18基质分散固相萃取净化,再经Acquity CSH氟苯基色谱柱(100 mm× 2.1 mm,1.7 μm)分离,串联质谱法检测,内标法定量.结果 高氯酸盐和氯酸盐在各自的线性范围内峰面积比与其质量浓度线性关系良好,相关系数(r)大于0.999;高氯酸盐和氯酸盐的检出限分别为0.2和1 μg/L,定量限为0.5和3 μg/L;两种化合物的平均回收率分别为84.0％～105.0％和82.7％～112.1％,相对标准偏差为4.2％～17.0％和5.5％～18.4％(n=6).11类饮料样品中高氯酸盐含量为0.53～4.12 μg/L,氯酸盐含量为3.27～61.86 μg/L.结论 本方法前处理简单、灵敏度高、准确、可靠,适用于饮料中高氯酸盐和氯酸盐的测定.
Abstract
OBJECTIVE To establish a method for determination of perchlorate and chlorate in drinks by ultra-performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)based on isotopic internal standard method.METHODS The perchlorate and chlorate residue in liquid drinks were extracted with methanol,in solid drinks with acetic acid solution,then centrifuged.The supernatant was cleaned-up with PSA/C18 cleanup tube.The separation of perchlorate and chlorate was carried out on a Acquity CSH fluorophenyl column(100 mm ×2.1 mm,1.7 μm)and the detection was performed with tandem mass spectrometry with internal standard method for quantification.RESULTS The peak area ratio of perchlorate and chlorate had a good linear relationship with their mass concentration within their respective linear ranges,with correlation.coefficients(r)greater than 0.999.The limits of detection of perchlorate and chlorate were 0.2 and 1 μg/L respectively and the limits of quantification were 0.5 and 3 μg/L respectively.The mean recoveries of two compounds were from 84.0％to 105.5％with relative standard deviations from 4.2％to 17.0％and 82.7％to 112.1％with relative standard deviations from 5.5％to 18.4％(n=6),respectively.The perchlorates in 11 kinds of beverage samples were 0.53-4.12 μg/L,chlorates were 3.27-61.86 μg/L.CONCLUSION This method is simple,sensitive,accurate and reliable,which is suitable for the determination of perchlorate and chlorate in drinks.
关键词
高氯酸盐/氯酸盐/同位素内标法/饮料/超高效液相色谱-串联质谱法Key words
perchlorate/chlorate/isotopic internal standard method/drinks/ultra performance liquid chromatography tandem mass spectrometry引用本文复制引用
基金项目
北京市科技计划(Z211100007021008)
高层次公共卫生技术人才培养计划(学科骨干-01-033)
出版年
2024
NETL
NSTL
维普
万方数据