超高效液相色谱串联-质谱法同时测定香辛料中7种真菌毒素
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摘要
建立了同时测定香辛料中7种真菌毒素的超高效液相色谱-串联质谱分析方法(UPLC-MS/MS)。选用香辛料中的辣椒、花椒和八角为研究对象,粉碎后的样品用70%甲醇水溶液提取,6合1免疫亲和柱净化,ACQUITY UPLC HSS T3色谱柱分离,超高效液相色谱-串联质谱测定,电喷雾正离子(ESI+)多反应离子监测方式监测,外标法定量。结果表明,7种真菌毒素在各自的线性响应范围内线性关系良好,相关系数均不低于0.995,7种真菌毒素的定量限为0.5～20μg/kg。低、中、高3个加标水平平均回收率(n=6)为67.25%～113.47%,相对标准偏差(RSD)为1.07%～10.20%。该方法具有前处理简单、净化效果好、灵敏度高和高通量检测的优点,适用于香辛料中多组分真菌毒素残留的分离和检测。
A method was developed for the determination of 7 mycotoxins in spices by ultra-high performance liquid chromatography-tendem mass spectrometry( UPLC-MS/MS).Selection of spices in chili,pepper and star anise for the study,smashed samples were extracted with 70% methanol water solution,purified by multifunction immunological affinity column,isolated by ACQUITY UPLC HSS T3 chromatographic column,determined by ultra-efficient liquid chromatography-mass spectrometry. The mass spectrometry was conducted by using positive( ESI+) electrospray ionization and multi-reactions monitoring( MRM) models,with external standard method.The results indicated that 7 mycotoxins had good linear relationship,correlation coefficient were not less than 0.995,and the limit of quantitation( LOQ) for the range from 0.5 to 20 μg/kg.The average recovery rates at three levels of adding external standard were from 67.25% to 113.47%,with a relative standard deviation( RSD)varying from 1.07% to 10.20%.The method had simple process,good purification effect and the advantages of high sensitivity and high throughput detection,suitable for spices in multicomponent separation and detection of mycotoxin residues.
A method was developed for the determination of 7 mycotoxins in spices by ultra-high performance liquid chromatography-tendem mass spectrometry( UPLC-MS/MS).Selection of spices in chili,pepper and star anise for the study,smashed samples were extracted with 70% methanol water solution,purified by multifunction immunological affinity column,isolated by ACQUITY UPLC HSS T3 chromatographic column,determined by ultra-efficient liquid chromatography-mass spectrometry. The mass spectrometry was conducted by using positive( ESI+) electrospray ionization and multi-reactions monitoring( MRM) models,with external standard method.The results indicated that 7 mycotoxins had good linear relationship,correlation coefficient were not less than 0.995,and the limit of quantitation( LOQ) for the range from 0.5 to 20 μg/kg.The average recovery rates at three levels of adding external standard were from 67.25% to 113.47%,with a relative standard deviation( RSD)varying from 1.07% to 10.20%.The method had simple process,good purification effect and the advantages of high sensitivity and high throughput detection,suitable for spices in multicomponent separation and detection of mycotoxin residues.
引文
[1]鲍蕾,梁成珠,刘学惠,等.出入境农产品中真菌毒素的污染、检测及控制[J]。中国食品工业,2005(1):60-61。
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[7]王玉娇,聂继云,闫震,等.超高效液相色谱-串联质谱法同时检测干果中16种真菌毒素[J].分析化学,2017,45(10):1556-1563.
[8]杨万颖,郑彦婕,李碧芳,等.液相色谱串联质谱法同时测定小麦粉中10种真菌毒素[J].广东化工,2008,35(9):123-128.
[9]葛宝坤,赵孔祥,王伟,等.免疫亲和柱净化-液相色谱-串联质谱法测定中药材中的14种真菌毒素[J].色谱,2011,29(6):495-500
[10]吴宇,叶金,张冰,等.稳定同位素稀释-超高效液相色谱-串联质谱法快速测定植物油中16种真菌毒素[J].分析化学,2018(6):975-984.
[11]李宁侠,唐招平,马宁.超高效液相色谱-质谱法同时检测中药酒剂中多种真菌毒素的污染水平[J].现代中药研究与实践,2017(2):57-61.
[12]勾金玉.粮谷饲料中多种真菌毒素残留同时检测方法的建立及应用研究[D].保定:河北农业大学,2013.
[13]王莎,孔维军,杨美华.同位素内标-超高效液相色谱串联质谱法检测麦芽中11种真菌毒素[J].药学学报,2016(1):110-115.
[14]王鹭,杨骅,谢国祥,等.普洱茶、红茶、绿茶中真菌毒素的检测[J].中国中药杂志,2017(24):4801-4806.
[15]李文廷,瑞雨,师真,等.桑椹中11种真菌毒素的检测分析[J].环境化学,2018(1):185-187.
[16]陈慧菲,朱天仪,陈凤香,等.QuEChERS-超高效液相色谱串联质谱法测定谷物中的8种真菌毒素[J].粮食与油脂,2016,29(5):67-70.
[17]郑荣,毛丹,王少敏,等.高效液相色谱-串联质谱法测定桃仁中10种真菌毒素[J].食品安全质量检测学报,2014(3):824-832.
[18]孙娟,李为喜,张妍,等.用超高效液相色谱串联质谱法同时测定谷物中12种真菌毒素[J].作物学报,2014,40(4):691-701.
[19]王晓春,汤奇峰,李鹏飞.高效液相色谱-三重四极杆串联质谱测定谷物中T-2毒素和HT-2毒素[J].分析试验室,2011,30(9):62-65.
[20]廉慧锋,赵笑天,王蓉珍,等.超高效液相色谱-串联质谱法同时测定玉米、花生、麦仁中的9种真菌毒素[J].食品科学,2010,31(20):360-366.
[2]Schatzmayr G,Zehner F,Tubel M,et al.Microbiologicals for deactivating mycotoxins[J].Molecular Nutrition and Food Research,2010,50(6):543-551..
[3]李新颖,石英,国际香辛料真菌毒素限量标准研究现状[J].中国调味品,2006(12):9-16。
[4]Kokkonen M K,Jestoi M N.A Multi-compound LC-MS/MSmethod for the screening of mycotoxins in grains[J].Food Analytical Methods,2009,2(2):128-140.
[5]Lattanzio V M,Solfrizzo M,Powers S,et al.Simultaneous determination of aflatoxins,ochratoxin A and Fusarium toxins in maize by liquid chromatography/tandem mass spectrometry after multitoxin immunoaffinity cleanup[J].Rapid Communications in Mass Spectrometry,2010,21(20):3253-3261.
[6]张晓飞,岳延涛,杨美华,等.色谱-质谱联用技术在真菌毒素检测中的研究进展[J].贵州农业科学,2009,37(12):109-114.
[7]王玉娇,聂继云,闫震,等.超高效液相色谱-串联质谱法同时检测干果中16种真菌毒素[J].分析化学,2017,45(10):1556-1563.
[8]杨万颖,郑彦婕,李碧芳,等.液相色谱串联质谱法同时测定小麦粉中10种真菌毒素[J].广东化工,2008,35(9):123-128.
[9]葛宝坤,赵孔祥,王伟,等.免疫亲和柱净化-液相色谱-串联质谱法测定中药材中的14种真菌毒素[J].色谱,2011,29(6):495-500
[10]吴宇,叶金,张冰,等.稳定同位素稀释-超高效液相色谱-串联质谱法快速测定植物油中16种真菌毒素[J].分析化学,2018(6):975-984.
[11]李宁侠,唐招平,马宁.超高效液相色谱-质谱法同时检测中药酒剂中多种真菌毒素的污染水平[J].现代中药研究与实践,2017(2):57-61.
[12]勾金玉.粮谷饲料中多种真菌毒素残留同时检测方法的建立及应用研究[D].保定:河北农业大学,2013.
[13]王莎,孔维军,杨美华.同位素内标-超高效液相色谱串联质谱法检测麦芽中11种真菌毒素[J].药学学报,2016(1):110-115.
[14]王鹭,杨骅,谢国祥,等.普洱茶、红茶、绿茶中真菌毒素的检测[J].中国中药杂志,2017(24):4801-4806.
[15]李文廷,瑞雨,师真,等.桑椹中11种真菌毒素的检测分析[J].环境化学,2018(1):185-187.
[16]陈慧菲,朱天仪,陈凤香,等.QuEChERS-超高效液相色谱串联质谱法测定谷物中的8种真菌毒素[J].粮食与油脂,2016,29(5):67-70.
[17]郑荣,毛丹,王少敏,等.高效液相色谱-串联质谱法测定桃仁中10种真菌毒素[J].食品安全质量检测学报,2014(3):824-832.
[18]孙娟,李为喜,张妍,等.用超高效液相色谱串联质谱法同时测定谷物中12种真菌毒素[J].作物学报,2014,40(4):691-701.
[19]王晓春,汤奇峰,李鹏飞.高效液相色谱-三重四极杆串联质谱测定谷物中T-2毒素和HT-2毒素[J].分析试验室,2011,30(9):62-65.
[20]廉慧锋,赵笑天,王蓉珍,等.超高效液相色谱-串联质谱法同时测定玉米、花生、麦仁中的9种真菌毒素[J].食品科学,2010,31(20):360-366.