硫酸磺化-同位素内标稀释-超高效液相色谱-串联质谱法快速筛查农作物中五氯酚及其钠盐残留被引量：1

Rapid determination of pentachlorophenol and its sodium salt residues in crops by sulfuric acid sulfonation-isotope internal standard dilution-ultra performance liquid chromatographytandem mass spectrometry

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摘要建立了一种快速分析筛查农作物中五氯酚及其钠盐残留的硫酸磺化-同位素内标稀释-超高效液相色谱-串联质谱法。通过调节样品pH值将样品中五氯酚钠转化成五氯酚后用正己烷提取,再进行磺化处理,采用超高效液相色谱串联质谱法进行测定,内标法定量。结果表明,五氯酚的质量浓度在0.15~10ng/mL范围内与色谱峰面积线性关系良好,相关系数大于0.999,方法检出限为0.15μg/kg,定量限为0.50μg/kg。样品的平均加标回收率为87%~108%,测定结果的相对标准偏差为2.11%~12.08%(n=6)。该方法操作简便且净化效果好,可用于食品安全风险监测中大批量样品快速分析筛查。 A method for the rapid analysis and screening of pentachlorophenol and its sodium salt residues in crops by sulfuric acid sulfonation-isotope internal standard dilution-ultra high performance liquid chromatography-tandem mass spectrometry was established.The sodium pentachlorophenol in the sample was converted into pentachlorophenol by adjusting the pH value of the sample,extracted with n-hexane,and then sulfonated.The ultra high performance liquid chromatography tandem mass spectrometry was used for determination,and the internal standard method was used for quantification.The results showed that the mass concentration of pentachlorophenol had a good linear relationship with the chromatographic peak area in the range of 0.15-10 ng/mL,and the correlation coefficient was greater than 0.999.The detection limit of the method was 0.15μg/kg,and the quantitative limit was 0.50μg/kg.The average spiked recoveries of the samples were 87%-108%,and the relative standard deviations of the determination results were 2.11%-12.08%(n=6).The method is simple and has good purification effect,which can be used for rapid analysis and screening of large quantities of samples in food safety risk monitoring.

作者黄圣南陈贻钢王显龙刘冬妮禤开智林正锋 HUANG Shengnan;CHEN Yigang;WANG Xianlong;LIU Dongni;XUAN Kaizhi;LIN Zhengfeng(Hainan Provincial Institute of Quality and Testing Food Testing Center,Key Laboratory of Tropical Fruits and Vegetables Quality and Safety,State Administration for Market Regulation,Haikou 570314,China;Haikou Customs Technical Center,Haikou 570311,China;Sanya Branch of Hainan Academy of Inspection and Testing,Sanya 572000,China)

机构地区海南省检验检测研究院食品检验检测中心海口海关技术中心海南省检验检测研究院三亚分所

出处《化学分析计量》 CAS 2024年第11期13-18,73,共7页 Chemical Analysis And Meterage

基金国家市场监督管理总局重点实验室(热带果蔬质量与安全)自主研究课题项目(ZZ-2024009)。

关键词农作物五氯酚及其钠盐磺化超高效液相色谱-串联质谱法内标法 crops pentachlorophenol and its sodium salts sulfonate ultra high performance liquid chromatography-tandem mass spectrometry internal standard method

分类号 O657.7 [理学—分析化学]

作者简介通信作者:刘冬妮,学士,食品工程师,主要从事食品质量安全检测研究。