广东化工2024，Vol.51Issue(17) ：185-187,213.DOI:10.3969/j.issn.1007-1865.2024.017.062

优化UPLC-MS/MS法和国标HPLC法对测定乳制品中三聚氰胺的对比研究

Comparative Study of Determination for Melamine in Dairy Products about Optimize Ultra Performance Liquid Chromatography Tandem Mass Spectrometry and High Performance Liquid Chromatography

吴锐滨 陈麒鹏 温映兰
广东化工2024，Vol.51Issue(17) ：185-187,213.DOI:10.3969/j.issn.1007-1865.2024.017.062
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  • 维普
  • 万方数据

优化UPLC-MS/MS法和国标HPLC法对测定乳制品中三聚氰胺的对比研究

Comparative Study of Determination for Melamine in Dairy Products about Optimize Ultra Performance Liquid Chromatography Tandem Mass Spectrometry and High Performance Liquid Chromatography

吴锐滨 1陈麒鹏 1温映兰1
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作者信息

  • 1. 广州检验检测认证集团有限公司,国家加工食品质量检验中心(广东),广东 广州 511447
  • 折叠

摘要

优化了测定乳制品中三聚氰胺的超高效液相色谱-串联质谱法(UPLC-MS/MS法),并与高效液相色谱法(HPLC法)进行比对实验,对两种检测方法的实验结果进行双总体t检验分析.样品经 1%高氯酸溶液和乙腈提取,高速离心分层,上清液用 PCX固相萃取柱进行净化,最后经 5%氨化甲醇洗脱并进行氮气浓缩,供UPLC-MS/MS测定.结果表明,HPLC法和UPLC-MS/MS法定量曲线方程的相关系数r2 均大于 0.995.在定量限 1 倍、2 倍和 10 倍的添加水平下,回收率分别为 87.8%～92.5%和89.8%～94.2%,相对标准偏差(RSD)为3.21%～5.24%和 5.05%～6.44%.两种方法检测结果之间无明显差异,优化后的UPLC-MS/MS法回收率更高,且重现性好,可应用于实际的日常样品检验中.

Abstract

The ultra high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)method for the determination of melamine in dairy products was optimized and comparative experiments on high performance liquid chromatography(HPLC)was conducted.A double population t-test analysis on the experimental results of two detection methods was performed.The sample was extracted with 1%perchloric acid solution and acetonitrile and separated by high-speed centrifugation,then the supernatant was purified using a PCX solid-phase extraction column.Finally,melamine was eluted with 5%ammoniated methanol and concentrated in nitrogen for UPLC-MS/MS determination.The results showed that the correlation coefficient r2 of the quantitative curve equations for both HPLC and UPLC-MS/MS methods were greater than 0.995.At the addition levels of 1,2,and 10 times the limit of quantification,the recoveries were 87.8%～92.5%and 89.8%～94.2%with relative standard deviation(RSD)of 3.21%～5.24%and 5.05%～6.44%,respectively.There is no significant difference in the detection results between the two methods.The optimized UPLC-MS/MS method has a higher recovery rate and good reproducibility,which can be applied to practical daily sample determination.

关键词

超高效液相色谱-串联质谱/高效液相色谱/乳制品/三聚氰胺/双总体t检验

Key words

UPLC-MS/MS/HPLC/dairy product/melamine/double population t-test

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出版年

2024
广东化工
广东省石油化工研究院

广东化工

影响因子：0.288
ISSN：1007-1865
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