超高效液相色谱-四极杆-飞行时间质谱法检测茶叶中玉米赤霉烯酮
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摘要
为探索检测茶叶中玉米赤霉烯酮的较佳方法,建立了发酵黑茶中玉米赤霉烯酮的超高效液相色谱-四极杆-飞行时间质谱(UPLC-Q-TOF-MS)检测方法。用甲醇水溶液(V(甲醇)∶V(水)=7∶3)提取玉米赤霉烯酮,以乙腈-水溶液为流动相,采用负模式,借助UPLC-Q-TOF-MS进行测定分析。玉米赤霉烯酮的质量浓度为0～1 000μg/L时,浓度与峰面积呈良好的线性关系;方法检出限(LOD,S/N≥3)为2μg/kg,定量下限(LOQ≥10)为6. 6μg/kg,相对标准偏差(RSD)为1. 3%～6. 8%;同时,不同茶叶样品的3个加标水平下,玉米赤霉烯酮的平均回收率为85. 6%～105. 5%。利用该方法检测32个黑茶样品中的玉米赤霉烯酮,结果显示,32个黑茶样品中的玉米赤霉烯酮的含量均低于国家标准,该方法操作简单、选择性好、灵敏度高,满足茶叶中玉米赤霉烯酮的测定要求。
For a better way to detect zearalenone in fermented dark tea,a method with ultra high performance liquid chromatography-MS quard-flight time mass spectrometry( UPLC-Q-TOF-MS) for detecting zearalenone in fermented dark tea was established.Zearalenone was extracted by using the solution of V( methanol) ∶V( water) = 7 ∶3,which was determined and analyzed using UPLC-Q-TOF-MS with acetonitrile and water as mobile phase and the negative model.The good linear relation between the peak area and the concentration was presented when the mass concentration range of zearalenone is 0 ～ 1 000 μg/L. The detecting limit( LOD,S/N≥3) is 2 μg/kg,the quantitative limit( LOQ≥10) is 6. 6 μg/kg,and the relative standard deviation( RSD) of1. 3% ～ 6. 8%.At the same time,the method was used to detect the zearalenone in 32 dark tea samples,the average recovery rate of the zearalenone in different samples is 85. 6% ～ 105. 5%. The results showed that the contents of zearalenone in 32 dark tea samples were below the national standard.This method is suitable for the requirements of determination of zearalenone in dark teas due to simple operation,good selection and high sensitivity.
For a better way to detect zearalenone in fermented dark tea,a method with ultra high performance liquid chromatography-MS quard-flight time mass spectrometry( UPLC-Q-TOF-MS) for detecting zearalenone in fermented dark tea was established.Zearalenone was extracted by using the solution of V( methanol) ∶V( water) = 7 ∶3,which was determined and analyzed using UPLC-Q-TOF-MS with acetonitrile and water as mobile phase and the negative model.The good linear relation between the peak area and the concentration was presented when the mass concentration range of zearalenone is 0 ～ 1 000 μg/L. The detecting limit( LOD,S/N≥3) is 2 μg/kg,the quantitative limit( LOQ≥10) is 6. 6 μg/kg,and the relative standard deviation( RSD) of1. 3% ～ 6. 8%.At the same time,the method was used to detect the zearalenone in 32 dark tea samples,the average recovery rate of the zearalenone in different samples is 85. 6% ～ 105. 5%. The results showed that the contents of zearalenone in 32 dark tea samples were below the national standard.This method is suitable for the requirements of determination of zearalenone in dark teas due to simple operation,good selection and high sensitivity.
引文
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[13]王桂芳,李培真,曹阳,等.胶体金测试条法对粮食中玉米赤霉烯酮快速定量测定的应用研究[J].粮食科技与经济,2014,1:32-34.
[14]王玉平,计融,江涛,等.玉米赤霉烯酮ELISA定量检测试剂盒研制[J].卫生研究,2006,2:221-224.
[15]孟卫芹,武玉香,唐世云,等.玉米油中玉米赤霉烯酮的ELISA测定[J].现代食品科技,2013,6(6):1 431-1 433.
[16]陈必芳,李兰.饲料中镰刀菌毒素DON、T-2和ZEN气相色谱测定方法研究[J].中国饲料,1995,10:32-34.
[17]鲍蕾,吕宁,吴振兴,等.免疫亲和柱同时净化-HPLC法测定植物油中黄曲霉毒素和玉米赤霉烯酮[J].食品工业科技,2013,34(9):306-309.
[18]谢刚,王松雪,崔华,等.超高效液相色谱法快速检测粮食中玉米赤霉烯酮的含量[J].粮油食品科技,2014,2:71-75.
[19]刘韬,王宁,杨璐,等.液相色谱-串联质谱技术检测多种基质中的三聚氰胺及10种真菌毒素[J].化学试剂,2017,39(12):1 305-1 310.
[20]姚婷,王丹,李双,等.超高效液相色谱-四级杆-飞行时间质谱法快速检测发酵黑茶中黄曲霉毒素B1[J].分析测试学报,2017,36(11):1 346-1 351.
[21]郭振,常靖,杨瑞琴,等.超高效液相色谱-四级杆-飞行时间质谱同时筛查腐败血液中24种农药[J].分析测试学报,2015,34(9):986-992.
[2]潘红艳.玉米赤霉烯酮在稻谷中的污染调查及毒理实验研究[D].武汉:武汉工业学院,2012.
[3]任丹丹,谢云峰,李少晖,等.饲料及食品中玉米赤霉烯酮检测方法研究进展[J].分析测试技术与仪器,2015,21(4):199-204.
[4]张明峰,王立明.大豆中抗营养因子的研究概况[J].大豆通报,1999,5:23-24.
[5]中华人民共和国国家卫生和计划生育委员会,国家食品药品监督管理总局.食品安全国家标准食品中真菌毒素限量:GB 2761—2017[S].2017-03-17.
[6]中华人民共和国国家质量监督检验检疫总局,中国国家标准化管理委员会.饲料卫生标准:GB 13078—2017[S].2017-10-14.
[7]胡琳玲,刘遵莹,刘秋玲,等.高效液相色谱法同时检测黑茶中16种多环芳烃化合物[J].茶叶科学,2014,34(4):324-330.
[8]王银诚,袁海波,江用文.黑茶品质成分及加工研究进展[J].中国农学通报,2016,32(22):194-199.
[9]吴永宁.现代食品安全科学[M].北京:化学工业出版社,2003:306-310.
[10]罗雪云,胡霞,李玉伟.小麦制品及玉米中玉米赤霉烯酮的薄层色谱测定[J].卫生研究,1993,2:112-115.
[11]杨小丽,杨美华,欧阳臻.玉米赤霉烯酮及其衍生物分析方法的研究进展[J].贵州农业科学,2011,7(7):234-238.
[12]牟钧,潘蓓,杨军,等.胶体金免疫层析法快速测定玉米和小麦中玉米赤霉烯酮[J].粮油食品科技,2011,5:43-45.
[13]王桂芳,李培真,曹阳,等.胶体金测试条法对粮食中玉米赤霉烯酮快速定量测定的应用研究[J].粮食科技与经济,2014,1:32-34.
[14]王玉平,计融,江涛,等.玉米赤霉烯酮ELISA定量检测试剂盒研制[J].卫生研究,2006,2:221-224.
[15]孟卫芹,武玉香,唐世云,等.玉米油中玉米赤霉烯酮的ELISA测定[J].现代食品科技,2013,6(6):1 431-1 433.
[16]陈必芳,李兰.饲料中镰刀菌毒素DON、T-2和ZEN气相色谱测定方法研究[J].中国饲料,1995,10:32-34.
[17]鲍蕾,吕宁,吴振兴,等.免疫亲和柱同时净化-HPLC法测定植物油中黄曲霉毒素和玉米赤霉烯酮[J].食品工业科技,2013,34(9):306-309.
[18]谢刚,王松雪,崔华,等.超高效液相色谱法快速检测粮食中玉米赤霉烯酮的含量[J].粮油食品科技,2014,2:71-75.
[19]刘韬,王宁,杨璐,等.液相色谱-串联质谱技术检测多种基质中的三聚氰胺及10种真菌毒素[J].化学试剂,2017,39(12):1 305-1 310.
[20]姚婷,王丹,李双,等.超高效液相色谱-四级杆-飞行时间质谱法快速检测发酵黑茶中黄曲霉毒素B1[J].分析测试学报,2017,36(11):1 346-1 351.
[21]郭振,常靖,杨瑞琴,等.超高效液相色谱-四级杆-飞行时间质谱同时筛查腐败血液中24种农药[J].分析测试学报,2015,34(9):986-992.