超高效液相色谱-串联质谱法测定4种浆果中5-硝基邻甲氧基苯酚钠和对硝基苯酚钠残留量  

Analysis of Sodium 5-nitroguaiacolate and Sodium Para-nitrophenolate Residues in Four Fruits by Usingultra-high Performance Liquid Chromatography-tandem Mass Spectrometry

作　　者：许旭[1,2,3,4] 侯雪 韩梅[2,3] 邱世婷 毛建霏[2,3] XU Xu;HOU Xue;HAN Mei;QIU Shi-ting;MAO Jian-fei(Chengdu Institute of Organic Chemistry Chinese Academy of Sciences,Sichuan Chengdu 610041,China;Center of Analysis and Testing,Sichuan Academy of Agricultural Sciences,Sichuan Chengdu 610066,China;Laboratory of Quality and Safety Risk Assessment for Agro-products (Chengdu),Ministry of Agriculture,Sichuan Chengdu 610066,China;University of Chinese Academy of Sciences,Beijing 100049,China)

机构地区：[1]中国科学院成都有机化学研究所,四川成都610041 [2]四川省农业科学院分析测试中心,四川成都610066 [3]农业部农产品质量安全风险评估实验室(成都),四川成都610066 [4]中国科学院大学,北京100049

出　　处：《西南农业学报》2019年第2期434-438,共5页Southwest China Journal of Agricultural Sciences

基　　金：2017年国家农产品质量安全风险评估项目(GJFP2017005)

摘　　要：【目的】为了测定浆果类水果(蓝莓、树莓、草莓及车厘子)中5-硝基对甲氧基苯酚钠(Sodium 5-nitroguaiacolate, 5NG)和对硝基苯酚钠(Sodium para-nitrophenolate, SD2)残留量,建立了快速测定5NG和SD2的超高效液相色谱-串联质谱(UPLC-MS/MS)检测方法。【方法】样品用乙腈提取,无需富集浓缩等特殊净化步骤,以CAPCELL PKA-C18色谱柱分离,采用电喷雾(ESI^-)-多反应监测模式(MRM)检测,基质匹配标准溶液外标法定量。【结果】在0.02～2.00 mg/kg范围内,5NG和SD2的质量浓度与对应的峰面积间线性关系良好,相关系数均大于0.9968。5-硝基对甲氧基苯酚钠和对硝基苯酚钠在浆果类水果(蓝莓、树莓、草莓及车厘子)中的检出限(LOD)别为0.28～0.73μg/kg,定量限(LOQ)为0.93～2.43μg/kg。在4个添加水平下,样品添加回收试验的平均回收率为91.75%～112.67%,相对标准偏差为1.07%～5.76%(n=6)。【结论】该方法简单快捷,灵敏度高,定量准确,可用于同时检测蓝莓、树莓、草莓及车厘子中5NG和SD2的残留量。【Objective】In order to determine the 5-nitroguaiacolate(5 NG)and sodium para-nitrophenolate residues(SD2)in berries(blueberry,raspberry,strawberry and cherry),a rapid method for analyzing 5 NG and SD2 by ultra-high performance liquid chromatography-electrospray ionization-tandem mass spectrometry(UPLC-ESI-MS/MS)was developed.【Method】The sample was extracted with acetonitrile,and no moreclean-up procedures were needed.Successful separation and detection were achieved on a CAPCELL PKA-C18 column and multiple reaction monitoring(MRM)in negative electrospray ionization(ESI^-)mode was used.【Result】Quantification was performed by peak area external standard methods using matrix-matched calibration curves,which were linear in the range of 0.02-2.00 mg/kg with good linear relationships.The correlation coefficients were all above 0.9968.The limits of detection(LOD)and limits of quantification(LOQ)for 5 NG and SD2 were 0.28-0.73 and 0.93-2.43μg/kg,respectively.At four spiked levels,the average recoveries ranged from 91.75%to 112.67%,and the relative standard deviation(n=6)was in the range of 1.07%-5.76%.【Conclusion】The method was quick,easy,sensitive,accurate and could be applied in the determination of 5 NG and SD2 residues in berries(blueberry,raspberry,strawberry and cherry).

关 键 词：超高效液相色谱-串联质谱 浆果 5-硝基对甲氧基苯酚钠 对硝基苯酚钠 

分 类 号：O657.63[理学—分析化学]