Determination of triforine residues in plant-derived food by solid phase extraction-high performance liquid chromatography-tandem mass spectrometry
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摘要: 建立了固相萃取-液相色谱-串联质谱测定植物源食品（大米、大豆、菠菜、番茄、辣椒、蘑菇等）中嗪氨灵残留量的检测方法。试样用乙腈均质提取,采用石墨化碳黑/氨基柱（ENVI-Carb/NH2）净化后,用多反应监测（MRM）正离子扫描方式进行检测,外标法定量。结果表明,嗪氨灵在21000 ng/m L范围内呈线性关系良好,方法的检出限（S/N=3）为0.51.5μg/kg,定量限（S/N=10）为1.64.9μg/kg,加标平均回收率范围为68.4%109.0%,相对标准偏差（RSD）为4.38%13.5%。方法的选择性好,抗干扰能力强,能满足国内外法规的要求,可以为植物源食品中嗪氨灵残留的检测提供技术支持。
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关键词:
- 高效液相色谱-串联质谱 /
- 嗪氨灵 /
- 固相萃取 /
- 植物源食品
Abstract: A method was developed for the simultaneous determination of triforine residue in various plant- derived foods( such as rice,soybean,spinach,tomato,pepper,and mushroom) by solid phase extraction- liquid chromatography- tandem mass spectrometry.The samples were extracted by acetonitrile,cleaned- up with an ENVI- Carb / NH2solid- phase extractor,and determined by high performance liquid chromatography- tandem mass spectrometry( HPLC- MS / MS) using external standard method with positive polarity mode under multi- reaction monitoring( MRM) scan type.The method showed good linearity in the range from 2 to 1000 ng / m L.The limits of detection( LODs,S / N = 3) varies over the range of 0.5 to 1.5 μg / kg,and limits of quantification( LOQs,S / N = 10) ranged from 1.6 to 4.9 μg / kg.The average recoveries in different matrices were in the range of68.4% ~109.0%,with relative standard deviations( RSDs) of 4.38% ~13.5%.This method was selective without interference and reliable for meeting the requirements of the domestic and international legislation. The method was suitable for triforine determination in plant- derived food.-
Keywords:
- HPLC-MS / MS /
- triforine /
- solid-phase extraction /
- plant-derived food
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[1] 潘建伟,祁彦,李淑娟,等.毛细管柱头衍生化气相色谱法测定水果、蔬菜中嗪氨灵残留量[J].检验检疫科学,2004,14(2):19-21. [2] 张宁,李洪,周游,等.嗪氨灵在西瓜土壤和西瓜中的降解动态和最终残留量[J].湖南农业大学学报:自然科学版,2013,39(3):298-303. [3] 陈武瑛,张德咏,李宗云,等.分散固相萃取-超高压液相色谱-串联质谱法测定黄瓜中的嗪氨灵[J].食品安全质量检测学报,2013,4(5):1511-1516. [4] 于彦彬,谭丕功,曲璐璐,等.PSA分散固相萃取液相色谱柱后衍生荧光法测定蔬菜和水果中的13中氨基甲酸酯[J].分析实验室,2009,28(11):97-101. [5] Ning Zhang,Hong Li,You Zhou,et al.Dissipation and residue of triforine in strawberry and soil[J].Environ Monit Assess,2014,186:1377-1384.
[6] 郭新东,冼燕萍,罗海英,等.气相色谱-三重串联四级杆质谱法测定粮谷中169种农药的残留量[J].现代食品科技,2012,28(6):695-702. [7] Guo-Fang Pang,Yong-Ming Liu,Chun-Lin Fan,et al.Simultaneous determiantion of 405 pesticied residues in grain by accelerated solvent extraction then gas chromatography-mass spectrometry or liquid chromatography-tandem mass spectrometry[J].Anal Bioanal Chem,2006,384:1366-1408.
[8] 丁明,钟冬莲,汤富彬,等.固相萃取-高效液相色谱-串联质谱联用测定竹笋中残留的7种杀虫剂农药[J].色谱,2013,31(2):117-121. [9] 徐娟,陈捷,王岚,等.Qu ECh ERS提取与超高效液相色谱-电喷雾电离串联质谱联用法检测果蔬中的230种农药残留[J].分析测试学报,2013,32(3):293-301. [10] 易盛国,候雪,韩梅,等.气相色谱-串联质谱法检测蔬菜农药残留基质效应与基质分类的研究[J].西南农业学报,2012,25(2):537-543. [11] 刘正才,杨方,余孔捷,等.液相色谱-电喷雾串联质谱法同时检测鸡组织中5种抗病毒类药物的残留量[J].色谱,2012,30(12):1253-1259. [12] Julie A H,Mark D S,Martin G,et al.Determination of triforine using high-performance liquid chromatography with tandem mass spectrometry[J].RCM,2004,18:775-779.
[13] 中华人民共和国国家进出口商品检验局中华人民共和国进出口商品检验行业标准.SN 0695-1997出口粮谷中嗪氨灵残留量检验方法[S].北京:中国标准出版社,1997.
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