文献类型：期刊文献

中文题名：QuEChERS结合超高效液相色谱-串联质谱法测定砂仁中4种黄曲霉毒素

英文题名：Identification of Four Aflatoxins in Fructus amomi using QuEChERS Combined with Ultra-performance Liquid Chromatography-tandem Mass Spectrometry

作者：陈昊文[1];周春霞[1];陈金[1];冼燕萍[2];管晶晶[1];胡均鹏[2];罗东辉[1,3]

机构：[1]广东海洋大学食品科技学院,广东海洋大学食品科学与工程学院,广东湛江524088;[2]广州质量监督检测研究院,广州市食品安全风险动态监测与预警研究中心,广州市食品安全检测技术重点实验室,广东广州511447;[3]化学与精细化工广东省实验室潮州分中心(韩江实验室),广东潮州521000

年份：2023

卷号：39

期号：12

起止页码：286

中文期刊名：现代食品科技

外文期刊名：Modern Food Science and Technology

收录：CSTPCD、、Scopus、北大核心、北大核心2020

基金：广东省重点领域研发计划项目(2021B070706001);潮州市重大科技创新项目(2020PT01);韩江实验室(HJL202101B005)。

语种：中文

中文关键词：超高效液相色谱-串联质谱(UPLC-MS/MS);黄曲霉毒素;砂仁

外文关键词：ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS);aflatoxin;Fructus amomi

中文摘要：该研究建立了利用QuEChERS-超高效液相色谱串联质谱(UPLC-MS/MS)法同时测定砂仁中4种黄曲霉毒素(Aflatoxin B1、B2、G1、G2)的分析方法。通过对QuEChERS前处理技术、色谱和质谱条件的优化,确定了最佳的实验条件。研磨后的样品经φ=1%甲酸酸化的乙腈提取,无水硫酸镁及氯化钠脱水盐析,上清液经十八烷基键合硅胶(C18)、乙二胺-N-丙基硅烷(PSA)、无水硫酸镁混合吸附剂净化。经ACQUITY UPLC HSS T3色谱柱(1.8μm,2.1 mm×100 mm)进行分离,以乙腈和φ=0.1%甲酸-5 mmol/L乙酸铵溶液进行梯度洗脱。在正离子模式下,进行多反应监测(MRM),进一步通过空白基质标准溶液外标法定量。结果表明,4种黄曲霉毒素在0.20~10.00μg/L范围内线性关系良好,相关系数均大于0.9989。实际样品的加标回收试验结果显示,回收率范围为89.50%~113.12%,日内精密度为1.31%~6.71%,日间精密度为1.29%~6.20%,4种黄曲霉毒素的方法检出限为0.30~0.60μg/kg、定量限为1.00~2.00μg/kg。该方法操作简单,快速,灵敏,适用于砂仁中4种黄曲霉毒素的定性、定量筛查。

外文摘要：A quick,easy,cheap,effective,rugged,and safe solid phase extraction(QuEChERS),in combination with ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)was established to identify four aflatoxins in Fructus amomi.Optimal experimental conditions were determined by optimizing the QuEChERS pre-treatment technique and the chromatographic and mass spectrometric conditions.The samples were extracted using acetonitrile with 1%formic acid and salted out with anhydrous magnesium sulfate and sodium chloride,then purified using C18,primary secondary amine(PSA),and magnesium sulfate anhydrous.The target analytes were separated on Waters HSS T3 columns(1.8μm,2.1 mm×100 mm),eluted by acetonitrile and a 0.1%(V/V)formic acid-5 mmol/L ammonium acetate solution gradient elution was used.Results were detected using MS/MS in positive ion mode under multiple reaction monitoring(MRM);quantification was further conducted using matrix-matched external standard calibrations.Good linearities for the four aflatoxins in the range of 0.20~10.00μg/L were obtained and the correlation coefficients were>0.9989.The recoveries were 89.50%~113.12%.The intraday relative standard deviations(Intra-RSDs)and interday relative standard deviations(Inter-RSDs)were 1.31%~6.71%and 1.29%~6.20%,respectively,as determined using spiked samples.The limits of detection and limits of quantification were 0.30~0.60μg/kg and 1.00~2.00μg/kg,respectively.The method is simple,rapid,and sensitive.It can be used for the qualitative determination and quantitative analysis of four aflatoxins residues in Fructus amomi.