超高压液相色谱-串联质谱法快速测定食品中多种真菌毒素含量的方法研究
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摘要
采用超高效液相色谱-串联质谱法,建立了超高效液相色谱-液质联用法同时测定食品中多种真菌毒素含量的检测方法。样品通过酸化乙腈提取,用七合一免疫亲和柱净化,通过Agilent Poroshell 120 EC-C18色谱柱分离,在正负离子多反应监测模式下分析定量。在1～10,5～50,10～100 ng/mL的质量浓度范围内线性良好,相关系数大于0.999,在5,10,20倍检出限添加水平下,平均回收率在75.9%～108.5%,相对标准偏差为4.9%～9.6%,方法检测限为0.2～10.0μg/kg,定量限为0.6～30.0μg/kg。
Application of ultra high performance liquid chromatography-tandem mass spectrometry,set up a method for simultaneous determination of mycotoxins in food by ultrahigh performance liquid chromatography-liquid mass spectrometry. Samples were extracted with acidic acetonitrile acidification,purified with a seven-in-one immunocompatibility column,and separated by Agilent Poroshell 120 EC-C18 chromatographic column. They were quantitatively analyzed in a multi-reaction monitoring mode of positive and negative ions. At concentrations ranging from 1～10,5～50,10～100 ng/mL,the correlation coefficient was greater than 0.999. At 5,10,20 times detection limit,the average recovery was 75.9%～108.5%,the relative standard deviation was 4.9%～9.6%,method detection limit was 0.2～10 μg/kg,the quantitative limit is 0.6～30 μg/kg.
Application of ultra high performance liquid chromatography-tandem mass spectrometry,set up a method for simultaneous determination of mycotoxins in food by ultrahigh performance liquid chromatography-liquid mass spectrometry. Samples were extracted with acidic acetonitrile acidification,purified with a seven-in-one immunocompatibility column,and separated by Agilent Poroshell 120 EC-C18 chromatographic column. They were quantitatively analyzed in a multi-reaction monitoring mode of positive and negative ions. At concentrations ranging from 1～10,5～50,10～100 ng/mL,the correlation coefficient was greater than 0.999. At 5,10,20 times detection limit,the average recovery was 75.9%～108.5%,the relative standard deviation was 4.9%～9.6%,method detection limit was 0.2～10 μg/kg,the quantitative limit is 0.6～30 μg/kg.
引文
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[4]王培,徐广超,尹丽梅,等.免疫亲和柱净化-高效液相色谱法同时检测小麦中脱氧雪腐镰刀菌烯醇及其衍生物[J].粮油食品科技,2015,23(1):63-66.
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[2]张思思,陆继伟,王少敏,等.国内外检测真菌毒素的标准及前处理研究进展[J].中国卫生检验杂志,2017,27(8):1 206-1 209.
[3]NY/T 1650-2008苹果及山楂制品中展青霉素的测定高效液相色谱法[S].北京:中国标准出版社,2008.
[4]王培,徐广超,尹丽梅,等.免疫亲和柱净化-高效液相色谱法同时检测小麦中脱氧雪腐镰刀菌烯醇及其衍生物[J].粮油食品科技,2015,23(1):63-66.
[5]陈建彪,董丽娜,刘娇,等. QuEChERs在食品中真菌毒素检测的研究进展[J].食品科学,2014,35(11):286-291.