大米中16种真菌毒素同时检测分析
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摘要
目的建立大米中黄曲霉毒素、伏马毒素、雪腐镰刀菌烯醇、脱氧雪腐镰刀菌烯醇类毒素、玉米赤霉烯酮、赭曲霉毒素A、T-2毒素、HT-2毒素以及杂色曲霉毒素等16种真菌毒素便捷准确的液相色谱-串联质谱法。方法大米样品经粉碎均质后采用70%甲醇水溶液浸泡提取,通过PriboFastRM226多功能净化柱净化,利用液相色谱串联质谱的多反应监测模式进行测定分析,采用内标法定量。结果 16种真菌毒素均具有良好的线性关系(r>0.99),3个加标水平回收率为85.2%～102.8%,相对标准偏差范围为2.05%～4.75%。在61件大米检测中,共有5件样品检出真菌毒素,检测到的真菌毒素有5种,其中雪腐镰刀菌烯醇、伏马毒素B_1、伏马毒素B_2、15-乙酰基脱氧雪腐镰刀菌烯醇各有1件样品检出,黄曲霉毒素B_1有3件检出,检出率为8.33%,检出的5种真菌毒素含量在0.69～71.47μg/kg,均未超过国家食品安全标准规定的真菌毒素限量标准。结论大米中真菌毒素的检出率低,含量符合国家标准要求,该检测方法准确、可靠、便捷,可适用于大米中多种真菌毒素的检测。
Objective To establish a convenient and accurate method for the determination of 16 mycotoxins,including aflatoxin, fumonisin, nivalenol, deoxynivalenol, zearalenone, ochratoxin A, T-2 toxin, HT-2 toxin and sterigmatocystin by liquid chromatography-tandem mass spectrometry. Methods Rice samples were extracted by 70% methanol aqueous solution after homogenization, purified by PriboFastRM226 multifunctional purification column, determined and analyzed by multi-reaction monitoring mode of liquid chromatography-tandem mass spectrometry, and quantified by internal standard method. Results The regression equations of 16 mycotoxins had good linear relationships(r > 0.99). The recoveries of the 3 spiked levels ranged from 85.2% to 102.8%, and the relative standard deviations ranged from 2.05% to 4.75%. In tests of 61 rice samples, 5 samples were found to detect mycotoxins, and 5 species of mycotoxins were detected. Among them, nivalenol, fumonisin B_1, fumonisin B_2,15-acetyl deoxynivalenol were detected in one sample, and aflatoxin B_1 was detected in 3 samples. The detection rate was 8.33%, and the five mycotoxins were detected in the range of 0.69-71.47 μg/kg, which did not exceed the limit of mycotoxin limit specified by the national food safety standards. Conclusion The detection rates of mycotoxins in rice are low, and the contents meet the requirements of national standards. The detection method is accurate, reliable and convenient, and can be applied to the detection of multiple mycotoxins in rice.
Objective To establish a convenient and accurate method for the determination of 16 mycotoxins,including aflatoxin, fumonisin, nivalenol, deoxynivalenol, zearalenone, ochratoxin A, T-2 toxin, HT-2 toxin and sterigmatocystin by liquid chromatography-tandem mass spectrometry. Methods Rice samples were extracted by 70% methanol aqueous solution after homogenization, purified by PriboFastRM226 multifunctional purification column, determined and analyzed by multi-reaction monitoring mode of liquid chromatography-tandem mass spectrometry, and quantified by internal standard method. Results The regression equations of 16 mycotoxins had good linear relationships(r > 0.99). The recoveries of the 3 spiked levels ranged from 85.2% to 102.8%, and the relative standard deviations ranged from 2.05% to 4.75%. In tests of 61 rice samples, 5 samples were found to detect mycotoxins, and 5 species of mycotoxins were detected. Among them, nivalenol, fumonisin B_1, fumonisin B_2,15-acetyl deoxynivalenol were detected in one sample, and aflatoxin B_1 was detected in 3 samples. The detection rate was 8.33%, and the five mycotoxins were detected in the range of 0.69-71.47 μg/kg, which did not exceed the limit of mycotoxin limit specified by the national food safety standards. Conclusion The detection rates of mycotoxins in rice are low, and the contents meet the requirements of national standards. The detection method is accurate, reliable and convenient, and can be applied to the detection of multiple mycotoxins in rice.
引文
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[6]高同春,王梅,段劲生,等.食品中真菌毒素的研究进展[C].食品安全的理论与实践-安徽食品安全博士科技论坛论文集,2008:735-745.Gao TC,Wang M,Duan JS,et al.Advance of studying on mycotoxins in food[C].Theory and practice of food safety--a collection of Doctoral Forum on Food Safety in Anhui,2008:735-745.
[7]刘峰良,赵志辉,谢晶.谷物中真菌毒素的研究进展[J].广东农业科学,2012,19:115-119.Liu FL,Zhao ZH,Xie J.Research progress of mycotoxins in cereals[J].Guangdong Agric Sci,2012,19:115-119.
[8]GB/T 2761-2017食品安全国家标准食品中真菌毒素限量[S].GB/T 2761-2017 National food safety standards-Limits of mycotoxins in food[S].
[9]GB 5009.111-2016食品安全国家标准食品中脱氧雪腐镰刀菌烯醇及其乙酰化衍生物的测定[S].GB 5009.111-2016 National food safety standard-Determination of deoxynivalenol and its acetylated derivatives in foods[S].
[10]GB 5009.209-2016食品安全国家标食品中玉米赤霉烯酮的测定[S].GB 5009.209-2016 National food safety standard-Determination of zearalenone in food[S].
[11]GB 5009.22-2016食品安全国家标准食品中黄曲霉毒素B族和G族的测定[S].GB 5009.22-2016 National food safety standard-Determination of aflatoxin B and G in food[S].
[12]GB 5009.240-2016食品安全国家标准食品中伏马毒素测定[S].GB 5009.240-2016 National food safety standard-Determination of fumonisin in food[S].
[13]李文廷,梁志坚,张瑞雨,等.超高效液相色谱-串联质谱法同时测定谷物及其制品中11种真菌毒素[J].食品安全质量检测学报,2018,8(10):3747-3755.Li WT,Liang ZJ,Zhang RY,et al.Determination of 11 kinds of mycotoxins in grains and its products by ultra performance liquid chromatography-tandem mass spectrometry[J].J Food Saf Qual,2018,8(10):3747-3755.
[14]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,2011,30:6-12.Gong XM,Ren YP,Dong J,et al.Determination of 18 mycotoxin contaminants in peanuts and oils by gel permeation chromatography and ultra performance liquid chromatography-tandem mass spectrometry[J].JInstrum Anal,2011,30:6-12.
[15]Frenich AG,Vidal JLM,Romero-Gonzalez R,et al.Simple and high-throughput method for the multimycotoxin analysis in cereals and related foods by ultra-high performance liquid chromatography tandem mass spectrometry[J].w Food Chem,2009,117:705-712.
[16]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,2014,4(4):691-701.Sun J,Li WX,Zhang Y,et al.Simultaneous determination of twelve mycotoxins in cereals by ultra-high performance liquid chromatography-tandem mass spectrometry[J].Acta Agron Sin,2014,4(4):691-701.
[17]郑翠梅,张艳,王松雪,等.液相谱-质谱联用同时检测粮食中多种真菌毒素的应用进展[J].粮食科技与经济,2012,37(1):45-49.Zheng CM,Zhang Y,Wang SX,et al.Study on application of a liquid chromatography-mass spectrometric technology in simultaneous determination of multi-mycotoxin in grain[J].Grain Sci Technol Econ,2012,37(1):45-49.
[18]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,2010,28:601-607.Meng J,Zhang J,Zhang N,et al.Determination of zearalenone and related mycotoxins in grain and its products by solid-phase extraction coupled with ultra performance liquid chromatography-tandem mass spectrometry[J].Chin J Chromatogr,2010,28:601-607.
[19]刘青,邹志飞,余炀炀,等.食品中真菌毒素法规限量标准概述[J].中国酿造,2017,36(1):12-18.Liu Q,Zou ZF,Yu YY,et al.Review of regulations of mycotoxins limit standard in foods[J].China Brew,2017,36(1):12-18.
[2]何健,冯民,朱臻怡,等.国外对真菌毒素的研究进展[J].农产品质量与安全,2013,1:72-74.He J,Feng M,Zhu ZY,et al.Advances in research on mycotoxins abroad[J].Qual Saf Agro-Product,2013,1:72-74.
[3]税丕容.食品中真菌毒素的污染与检测研究进展[J].现代食品,2018,13:131-136.Shui PR.Research progress on contamination and detection of mycotoxins in foods[J].Mod Food,2018,13:131-136.
[4]杨世亚,邱景富.食品中真菌毒素的污染状况与检测方法研究进展[J].现代预防医学,2012,22:5897-5900.Yang SY,Qiu JF.Research progress of pollution condition and detecting methods in mycotoxins in the food[J].Mod Prev Med,2012,22:5897-5900.
[5]马皎洁,邵兵,林肖惠,等.我国部分地区2010年产谷物及其制品中多组分真菌毒素污染状况研究[J].中国食品卫生杂志,2011,23(6):481-488.Ma JJ,Shao B,Lin XH,et al.Study on the natural occurrence of multi-mycotoxin in cereal and cereal-based product samples collected from parts of China in 2010[J].Chin J Food Hyg,2011,23(6):481-488.
[6]高同春,王梅,段劲生,等.食品中真菌毒素的研究进展[C].食品安全的理论与实践-安徽食品安全博士科技论坛论文集,2008:735-745.Gao TC,Wang M,Duan JS,et al.Advance of studying on mycotoxins in food[C].Theory and practice of food safety--a collection of Doctoral Forum on Food Safety in Anhui,2008:735-745.
[7]刘峰良,赵志辉,谢晶.谷物中真菌毒素的研究进展[J].广东农业科学,2012,19:115-119.Liu FL,Zhao ZH,Xie J.Research progress of mycotoxins in cereals[J].Guangdong Agric Sci,2012,19:115-119.
[8]GB/T 2761-2017食品安全国家标准食品中真菌毒素限量[S].GB/T 2761-2017 National food safety standards-Limits of mycotoxins in food[S].
[9]GB 5009.111-2016食品安全国家标准食品中脱氧雪腐镰刀菌烯醇及其乙酰化衍生物的测定[S].GB 5009.111-2016 National food safety standard-Determination of deoxynivalenol and its acetylated derivatives in foods[S].
[10]GB 5009.209-2016食品安全国家标食品中玉米赤霉烯酮的测定[S].GB 5009.209-2016 National food safety standard-Determination of zearalenone in food[S].
[11]GB 5009.22-2016食品安全国家标准食品中黄曲霉毒素B族和G族的测定[S].GB 5009.22-2016 National food safety standard-Determination of aflatoxin B and G in food[S].
[12]GB 5009.240-2016食品安全国家标准食品中伏马毒素测定[S].GB 5009.240-2016 National food safety standard-Determination of fumonisin in food[S].
[13]李文廷,梁志坚,张瑞雨,等.超高效液相色谱-串联质谱法同时测定谷物及其制品中11种真菌毒素[J].食品安全质量检测学报,2018,8(10):3747-3755.Li WT,Liang ZJ,Zhang RY,et al.Determination of 11 kinds of mycotoxins in grains and its products by ultra performance liquid chromatography-tandem mass spectrometry[J].J Food Saf Qual,2018,8(10):3747-3755.
[14]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,2011,30:6-12.Gong XM,Ren YP,Dong J,et al.Determination of 18 mycotoxin contaminants in peanuts and oils by gel permeation chromatography and ultra performance liquid chromatography-tandem mass spectrometry[J].JInstrum Anal,2011,30:6-12.
[15]Frenich AG,Vidal JLM,Romero-Gonzalez R,et al.Simple and high-throughput method for the multimycotoxin analysis in cereals and related foods by ultra-high performance liquid chromatography tandem mass spectrometry[J].w Food Chem,2009,117:705-712.
[16]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,2014,4(4):691-701.Sun J,Li WX,Zhang Y,et al.Simultaneous determination of twelve mycotoxins in cereals by ultra-high performance liquid chromatography-tandem mass spectrometry[J].Acta Agron Sin,2014,4(4):691-701.
[17]郑翠梅,张艳,王松雪,等.液相谱-质谱联用同时检测粮食中多种真菌毒素的应用进展[J].粮食科技与经济,2012,37(1):45-49.Zheng CM,Zhang Y,Wang SX,et al.Study on application of a liquid chromatography-mass spectrometric technology in simultaneous determination of multi-mycotoxin in grain[J].Grain Sci Technol Econ,2012,37(1):45-49.
[18]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,2010,28:601-607.Meng J,Zhang J,Zhang N,et al.Determination of zearalenone and related mycotoxins in grain and its products by solid-phase extraction coupled with ultra performance liquid chromatography-tandem mass spectrometry[J].Chin J Chromatogr,2010,28:601-607.
[19]刘青,邹志飞,余炀炀,等.食品中真菌毒素法规限量标准概述[J].中国酿造,2017,36(1):12-18.Liu Q,Zou ZF,Yu YY,et al.Review of regulations of mycotoxins limit standard in foods[J].China Brew,2017,36(1):12-18.