基质分散固相萃取-液质联用法测定食用香精香料中的黄曲霉素类真菌毒素
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- 英文论文题名：Determination of the aflatoxin class mycotoxins in edible essence by matrix solid-phase dispersionextraction--highperformance liquid chromatography-tandem mass spectrometry
- 论文作者：王冲 ; 孙海峰 ; 吕乔 ; 陈嘉彬 ; 王奕 ; 谢涛
- 英文论文作者：Wang Chong ; Sun Hai-feng ; Lv Qiao ; Chen Jia-bin ; Zhang Liang ; Wang Yi ; Xie Tao ; Technology center of Shenzhen Tobacco Industry Co. ; Ltd
- 年：2016
- 作者机构：深圳烟草工业有限责任公司技术中心;
- 论文关键词：高效液相色谱-串联质谱 ; 香精 ; 黄曲霉毒素 ; 分散固相萃取
- 英文论文关键词：Aflatoxins ; Mycotoxins ; Edible essence ; HPLC-MS/MS ; Matrix solid-phase dispersion
- 会议召开时间：2016-12-01
- 会议录名称：中国烟草学会2016年度优秀论文汇编——卷烟材料主题
- 语种：中文
- 分类号：TS264.3;O657.63
- 学会代码：ZGYG
- 学会名称：中国烟草学会
- 页数：9
- 文件大小：1199k
- 原文格式：D
摘要
建立了高效液相色谱-串联质谱法(HPLC-MS/MS)同时测定食用香精中的四种黄曲霉素类真菌毒素的方法。食用香精样品用甲醇-水(84:16,V/V)萃取,提取液经ODS C18分散固相萃取净化,采用HPLC-MS/MS进行色谱柱分析。待测物标准品在0.1~30μg/L浓度范围内线性关系良好,相关系数r>0.991;B1、B2、G1和G2定量限(LOQ)分别为0.28、0.36、0.41和0.22μg/kg,回收率在61.4%~116.9%之间,相对标准偏差(RSD)在4.5%~11.9%之间。结果表明,该方法灵敏度高、选择性强且稳定性好,可用于食用香精中黄曲霉素类真菌毒素的检测。
An easy method for the determination of Aflatoxin class mycotoxins in edible essence by highperformance liquid chromatography coupled with tandem mass spectrometry(HPLC-MS/MS) has beendeveloped. Edible essence samples were extracted with methanol-water(84:16, V/V) and then it was purified by ODS C18 matrix solid-phase dispersion, and the extracts were determined by HPLC-MS/MS. The good correlation coefficients(r>0.991) of thefour aflatoxins were obtained within their respective linear ranges(0.1~30μg/L). The determinationlimits for 4 kinds of aflatoxins were 0.28、 0.36、 0.41、0.22 μg/kg,the average recoveries were between61.4 %~116.9%, the relative standard deviations(RSD) were in the range from 4.5% to11.9 %. The resultsindicated that the developed method is sensitive, fast, accurate, and can be applied for the determinationof theaflatoxin class mycotoxins in edible essence samples.
An easy method for the determination of Aflatoxin class mycotoxins in edible essence by highperformance liquid chromatography coupled with tandem mass spectrometry(HPLC-MS/MS) has beendeveloped. Edible essence samples were extracted with methanol-water(84:16, V/V) and then it was purified by ODS C18 matrix solid-phase dispersion, and the extracts were determined by HPLC-MS/MS. The good correlation coefficients(r>0.991) of thefour aflatoxins were obtained within their respective linear ranges(0.1~30μg/L). The determinationlimits for 4 kinds of aflatoxins were 0.28、 0.36、 0.41、0.22 μg/kg,the average recoveries were between61.4 %~116.9%, the relative standard deviations(RSD) were in the range from 4.5% to11.9 %. The resultsindicated that the developed method is sensitive, fast, accurate, and can be applied for the determinationof theaflatoxin class mycotoxins in edible essence samples.
引文
[1]谢剑平.烟草香料技术原理与应用[M].北京:化学工业出版社,2009:74-78.
[2]李鹏,赖卫华,金晶.食品中真菌毒素的研究[J].农产品加工,2005,34(3):12-15.
[3]张艺兵,鲍蕾,褚庆华.农产品中真菌毒素的检测分析[M].北京:化学工业出版社,2006:15.
[4]Thrane U.Fusarium:mycotoxins,taxonomy and pathogenicity[M].Amsterdam:Elsevier,1989:199.
[5]Arora K A.Handbook of applied mycology[M].New York:Marcel Dekker,1992:87.
[6]Betina V.Mycotoxins:chemical,biological and environmentalaspects[M].Amsterdam:Elsevier,1989:56.
[7]Elisabete Y.S,Mario A,Fabia Y,et al.Evaluation of fumonisimaflatoxinco-occurrence in Brazilian cornhybrids by ELISA[J].Food Addit.Contam.,2001,18(8):719-729.
[8]王彩云,王政纲,云战友.酶联免疫法测定食品和饲料中的黄曲霉毒素[J].食品工程,2007(4):58-60.
[9]张海涛,徐燕飞,袁艺.不同前处理方法对饲草中黄曲霉素B1测定的影响[J].中国奶牛,2013(11):12-14.
[10]孔祥虹,高军刚等.超高效液相色谱-串联质谱法测定植物提取物中的4种黄曲霉毒素[J].食品科技,2013(04):325-329.
[11]郑润生,肖启衍,邱薇等.10种中药材和3种食品污染赭曲霉毒素A的LC-MS/MS检测研究[J].药物分析杂志,2015(2):289-294.
[12]Meritxell Ventura,Antonio G’omez,Ivan Anaya,et al.Determination of aflatoxins B1,G1,B2,and G2in medicinal herbs by liquid chromatography-tandem mass spectrometry[J].Journal of Chromatography A,2004,1048:25-29.
[13]Michael Sulyok,Franz Berthiller.Development and validation of a liquid chromatographytandem mass spectrometric method for the determinationof 39 mycotoxins in wheat and maize[J].Rapid Column.Mass Spectrom.2006,20:2649-2659.
[14]Antonia GarridoF renich,JoséLuis Martínez Vidal,Roberto Romero-González.Simple and high-throughput method for the multimycotoxin analysis in cerealsand related foods by ultra-high performance liquid chromatography/tandemmass spectrometry[J].Food Chemistry 2009(117):705-712.
[15]廉慧峰,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中真菌毒素[J].食品科学,2010,31(20):360-366.
[16]康绍英,周兴旺,张继红等.液相色谱--串联质谱法同时检测食品中的4中黄曲霉毒素[J].食品与机械,2013(2):77-82.
[17]GB/T 5009.23-2006食品中黄曲霉毒素G1、G2、B1、B2的测定[S].
[18]饲料中黄曲霉毒素、玉米赤霉烯酮和T-2毒素的测定液相色谱--串联质谱法[S],NY/T 2071-2011.
[19]郑翠梅,张燕,王松雪等.液相色谱-飞行时间质谱同时测定粮食中的13种真菌毒素[J].分析测试学报,2012(4):383-389.
[20]赵孔祥,胡筱芸,何佳等.免疫亲和净化-液相色谱--串联质谱测定中成药中14个真菌毒素[J].药物分析杂志,2012,32(5):846-851.
[21]孟娟,张晶,张楠等.固相萃取-超高效液相色谱-串联质谱法检测粮食及其制品中的玉米赤霉烯酮类真菌毒素[J].色谱,2010,28(6):601-607.
[22]闫龙宝,王浩,液相色谱-质谱联用技术测定葡萄酒中的赭曲霉毒素A残留[J].食品开发与研究,2010,31(6):136-138.
[23]宫小明,任一平,董静等.超高效液相色谱串联质谱法测定花生、粮油中18种真菌毒素[J].分析测试学报,2011,30(1):6-12.
[24]徐春祥,王超,舒婷等.串联四级杆液质联用测定粮食中8种真菌毒素[J].江苏农业科学,2010(6):494-496.
[25]Sulyok M,Krska R,Schuhmacher R.A liquidchromatography/tandem mass spectrometric multi-mycotoxin methodfor the quantification of 87 analytes and its application to semi-quantitative screening of moldy food samples[J].Analytical and Bioanalytical Chemistry,2007,389(5):1505-1523.
[26]Blesa J,Soriano J.M,Molto J.C.Determination of aflatoxins in peanuts by matrix solid-phase dispersion and liquud chromatography,Journal of chromatography A[J].2003(1011):49-54.
[27]Rubert J,Soler C,Manes J.Optimization of Matrix Solid-Phase Dispersion Method for simultaneous extraction of aflatoxins and OTA in cereals and its application to commercial samples.Talanta[J].2010(82):567-574.
[28]Barker SA.Applications of Matrix Solid-Phase dispersion in food analysis,Journal of Chromatography A[J].2000(880):63-68.
[29]GB2761-2011食品安全国家标准食品中真菌毒素限量[S].
[2]李鹏,赖卫华,金晶.食品中真菌毒素的研究[J].农产品加工,2005,34(3):12-15.
[3]张艺兵,鲍蕾,褚庆华.农产品中真菌毒素的检测分析[M].北京:化学工业出版社,2006:15.
[4]Thrane U.Fusarium:mycotoxins,taxonomy and pathogenicity[M].Amsterdam:Elsevier,1989:199.
[5]Arora K A.Handbook of applied mycology[M].New York:Marcel Dekker,1992:87.
[6]Betina V.Mycotoxins:chemical,biological and environmentalaspects[M].Amsterdam:Elsevier,1989:56.
[7]Elisabete Y.S,Mario A,Fabia Y,et al.Evaluation of fumonisimaflatoxinco-occurrence in Brazilian cornhybrids by ELISA[J].Food Addit.Contam.,2001,18(8):719-729.
[8]王彩云,王政纲,云战友.酶联免疫法测定食品和饲料中的黄曲霉毒素[J].食品工程,2007(4):58-60.
[9]张海涛,徐燕飞,袁艺.不同前处理方法对饲草中黄曲霉素B1测定的影响[J].中国奶牛,2013(11):12-14.
[10]孔祥虹,高军刚等.超高效液相色谱-串联质谱法测定植物提取物中的4种黄曲霉毒素[J].食品科技,2013(04):325-329.
[11]郑润生,肖启衍,邱薇等.10种中药材和3种食品污染赭曲霉毒素A的LC-MS/MS检测研究[J].药物分析杂志,2015(2):289-294.
[12]Meritxell Ventura,Antonio G’omez,Ivan Anaya,et al.Determination of aflatoxins B1,G1,B2,and G2in medicinal herbs by liquid chromatography-tandem mass spectrometry[J].Journal of Chromatography A,2004,1048:25-29.
[13]Michael Sulyok,Franz Berthiller.Development and validation of a liquid chromatographytandem mass spectrometric method for the determinationof 39 mycotoxins in wheat and maize[J].Rapid Column.Mass Spectrom.2006,20:2649-2659.
[14]Antonia GarridoF renich,JoséLuis Martínez Vidal,Roberto Romero-González.Simple and high-throughput method for the multimycotoxin analysis in cerealsand related foods by ultra-high performance liquid chromatography/tandemmass spectrometry[J].Food Chemistry 2009(117):705-712.
[15]廉慧峰,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中真菌毒素[J].食品科学,2010,31(20):360-366.
[16]康绍英,周兴旺,张继红等.液相色谱--串联质谱法同时检测食品中的4中黄曲霉毒素[J].食品与机械,2013(2):77-82.
[17]GB/T 5009.23-2006食品中黄曲霉毒素G1、G2、B1、B2的测定[S].
[18]饲料中黄曲霉毒素、玉米赤霉烯酮和T-2毒素的测定液相色谱--串联质谱法[S],NY/T 2071-2011.
[19]郑翠梅,张燕,王松雪等.液相色谱-飞行时间质谱同时测定粮食中的13种真菌毒素[J].分析测试学报,2012(4):383-389.
[20]赵孔祥,胡筱芸,何佳等.免疫亲和净化-液相色谱--串联质谱测定中成药中14个真菌毒素[J].药物分析杂志,2012,32(5):846-851.
[21]孟娟,张晶,张楠等.固相萃取-超高效液相色谱-串联质谱法检测粮食及其制品中的玉米赤霉烯酮类真菌毒素[J].色谱,2010,28(6):601-607.
[22]闫龙宝,王浩,液相色谱-质谱联用技术测定葡萄酒中的赭曲霉毒素A残留[J].食品开发与研究,2010,31(6):136-138.
[23]宫小明,任一平,董静等.超高效液相色谱串联质谱法测定花生、粮油中18种真菌毒素[J].分析测试学报,2011,30(1):6-12.
[24]徐春祥,王超,舒婷等.串联四级杆液质联用测定粮食中8种真菌毒素[J].江苏农业科学,2010(6):494-496.
[25]Sulyok M,Krska R,Schuhmacher R.A liquidchromatography/tandem mass spectrometric multi-mycotoxin methodfor the quantification of 87 analytes and its application to semi-quantitative screening of moldy food samples[J].Analytical and Bioanalytical Chemistry,2007,389(5):1505-1523.
[26]Blesa J,Soriano J.M,Molto J.C.Determination of aflatoxins in peanuts by matrix solid-phase dispersion and liquud chromatography,Journal of chromatography A[J].2003(1011):49-54.
[27]Rubert J,Soler C,Manes J.Optimization of Matrix Solid-Phase Dispersion Method for simultaneous extraction of aflatoxins and OTA in cereals and its application to commercial samples.Talanta[J].2010(82):567-574.
[28]Barker SA.Applications of Matrix Solid-Phase dispersion in food analysis,Journal of Chromatography A[J].2000(880):63-68.
[29]GB2761-2011食品安全国家标准食品中真菌毒素限量[S].