小麦粉中脱氧雪腐镰刀菌烯醇(DON)毒素的气相色谱法检测及毒素污染去除分析
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摘要
建立了一种用气相色谱仪分析小麦粉中脱氧雪腐镰刀菌烯醇(DON)毒素残留的分析方法。样品以乙腈/水混合溶液提取,样品提取液经充分晾干后,将毒素生成三甲基硅烷(TMS)衍生物,最后用电子捕获检测器(ECD)测定。DON在0.01～1.0mg/L范围内线性关系良好,线性相关系数为0.998 5。在0.04、0.2、1.0 mg/kg 3个浓度水平进行了添加实验,在小麦粉中其平均回收率为93.8%～108.5%,相对标准偏差为4.3%～8.6%。方法的最低检测浓度为0.01 mg/kg。该方法操作简单、快速、准确,可普遍用于基层检测机构中小麦粉DON的日常检测。结果表明:面粉中DON含量明显低于小麦粒中,对田间看似健康的小麦粒是否感染DON毒素,是无法简单通过肉眼观察到的,所以对小麦粒进行DON含量监测和去毒处理是非常有必要的。
A method for the determination of deoxynivalenol( DON) residues in flour by gas chromatography was developed. The sample was extracted with acetonitrile/water mixture. After the sample was dried completely, the toxin was derived into three methyl silane(TMS) derivative,and finally determined by electron capture detector(ECD). The calibration curves were of good linearity in the range of 0. 01 ～1.0 mg/L( R = 0. 998 5). The limit of quantification of the method was 0. 01 mg/kg. The average recoveries were between 93. 8% ～108. 5% at three spiked levels(0. 04、0. 2、1. 0 mg/kg) with the relative standard deviations( RSDs) in the range of 4. 3% ～8. 6%. The method is simple, rapid and accurate enough to be used for the routine analysis of DON in wheat flour at basic-level inspection organizations. The results showed that the content of DON in wheat flour was much lower than that in wheat grain in the field. The wheat grain in the field which appears healthy, cannot be determined only by the naked eye if it is infected with DON toxin. Therefore, it is essential to monitor DON Content in wheat and detoxify wheat grain.
A method for the determination of deoxynivalenol( DON) residues in flour by gas chromatography was developed. The sample was extracted with acetonitrile/water mixture. After the sample was dried completely, the toxin was derived into three methyl silane(TMS) derivative,and finally determined by electron capture detector(ECD). The calibration curves were of good linearity in the range of 0. 01 ～1.0 mg/L( R = 0. 998 5). The limit of quantification of the method was 0. 01 mg/kg. The average recoveries were between 93. 8% ～108. 5% at three spiked levels(0. 04、0. 2、1. 0 mg/kg) with the relative standard deviations( RSDs) in the range of 4. 3% ～8. 6%. The method is simple, rapid and accurate enough to be used for the routine analysis of DON in wheat flour at basic-level inspection organizations. The results showed that the content of DON in wheat flour was much lower than that in wheat grain in the field. The wheat grain in the field which appears healthy, cannot be determined only by the naked eye if it is infected with DON toxin. Therefore, it is essential to monitor DON Content in wheat and detoxify wheat grain.
引文
[1]GB 2761-2011.食品安全国家标准——食品中真菌毒素限量[S].北京:中华人民共和国卫生部,2011.
[2]胡绪英,王令春,曹金鸿,等.谷物中脱氧雪腐镰刀菌烯醇和雪腐镰刀菌烯醇的气相色谱分析[J].环境化学,1989,8(4):1-5.
[3]魏润蕴,王竹天.谷物中脱氧雪腐镰刀菌烯醇和雪腐镰刀菌烯醇的气相色谱测定[J].卫生研究,1996,25(4):242-245.
[4]黄志兵,游淑珠,邓舜洲,等.毛细管气相色谱法测定小麦和玉米中脱氧雪腐镰刀菌烯醇[J].食品科学,2007,28(4):241-245.
[5]唐吉旺,周丛,林源,等.毛细管-气相色谱法测定谷物中脱氧雪腐镰刀菌烯醇和雪腐镰刀菌烯醇的含量[J].理化检验-化学分册,2012,48(12):1441-1443.
[6]马立新.气相色谱仪测定进口小麦中镰刀菌毒素DON和NIV[J].中国国境卫生检疫杂志,1990,13(6):363-365.
[7]Tacke B K,Casper H H.Determination of Dexynivalenol in wheat,barley,and malt by column cleanup and gas chromatography with electron capture detection[J].Journal of AOAC international,1996,79(2):472-475.
[8]裴自友,韩航如,李亚浩,等.两种检测小麦中DON含量方法的比较与应用[J].麦类作物学报,2006,26(5):153-158.气质-液相
[9]ARIKA J,AIBERTO R,AND A.Analysis of the fusarium mycotetxius fusapmli&rin and trichothecenes in grai-ns using gas chromatography-mass spectrometry.[J]Ac Foos Chem,2004,52:1464-1469.气质
[10]隋凯,李军,卫锋.多功能净化-高效液相色谱法同时检测小麦中雪腐镰刀烯醇和脱氧雪腐镰刀烯醇[J].分析测试学报,2006,25(3):56-59.
[11]朱孟丽.高效液相色谱法对谷物汇总呕吐毒素的测定[J].粮食与饲料工业,2005,8:42-43.
[12]隋凯,李军,卫锋,等.谷物中脱氧雪腐镰刀菌烯醇的高效液相色谱检测及质谱确证[J].分析化学研究简报,2005,11(33):1643-1646.
[13]杨丹,耿志明,马鸿翔,等.高效液相色谱-紫外法同时检测小麦中DON、15ACDON和3ACDON[J].作物学报,2011,38(1):186-189.
[14]罗颖鹏,陈正行,王韧,等.固相萃取柱净化-高效液相色谱法测定小麦中脱氧雪腐镰刀菌烯醇[J].食品科学,2015,36(20):222-225.
[15]吴杰,陈万权,朱宝成.利用单克隆免疫亲和柱——高效液相色谱法检测小麦中DON毒素的研究[J].畜牧与饲料科学,2009,30(4):10-11.
[16]王伟,刘安法,李明奇,等.免疫亲和柱净化——高效液相色谱法检测小麦中脱氧雪腐镰刀菌烯醇[J].粮食与饲料工业,2013,1:60-61.
[17]欧阳毅,程树峰,唐芳,等.小麦脱氧雪腐镰刀菌烯醇(DON)检测方法的研究[J].粮油食品科技,2015,23(3):69-72.
[18]杨丹妮,汪海峰.小麦中呕吐毒素的ELISA和HPLC法检测[J].安徽农业科学,2013,41(3):1269-1270.
[19]龚燕,孙秀兰,邵景东.酶联免疫法检测呕吐毒素的方法研究[J].食品科学,2007,28(10):473-476.
[20]吴茂森,何晨阳.小麦赤霉病穗组织中黄色镰刀菌和DON毒素的定量分析[J].植物保护学报,2008,35(1):33-36.
[21]Usleber E,Erwin Martlbauer,Dietrich R,et al.Direct enzyme—linked immunosorbent assays for the detection of the 8-ketotriehothecene mycotoxins deoxynivalenol,3-acetyldeoxyivalenol,and 15-acetyldeoxyivalenol in buffer solutions.J Agric Food Chem,1991,39(11):2091-2095.
[22]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].北京: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,2016.
[23]Biselli S,Hummert C.Development of a multi-component method for Fusarium toxins using LC-MS/MSand its application during a survey for the content oft-2toxin and Dexynivalenol in various feed and food samples[J].Food additives&contaminants,2005,22(8):752-760.
[24]金海涛,张晓波,任红波,等.高效液相色谱质谱法快速测定小麦中DON、ZON、T-2的残留方法研究[J].粮食加工,2016,41(1):73-75.
[25]黄娟,陈国松,张晓燕,等.固相萃取-高效液相色谱-串联质谱法检测粮食及其制品中的呕吐毒素[J].色谱,2012,30(11):1203-1207.
[26]樊平声,沙国栋,张勇,等.南京市售小麦食品中DON毒素含量调查与风险评估[J].山地农业生物学报,2009,28(5):421-424.
[27]张祎,刘珊珊.江苏小麦生长期呕吐毒素监测预警研究进展[J].现代面粉工业,2016,1:21-22.
[28]白艺珍,李培武,丁小霞,等.我国粮油作物产品真菌毒素风险评估现状与对策研讨[J].农产品质量与安全,2015,5:54-58.
[29]张慧杰.小麦真菌毒素在加工过程中的消解、转移规律研究[D].北京,中国农业科学院,2014.
[2]胡绪英,王令春,曹金鸿,等.谷物中脱氧雪腐镰刀菌烯醇和雪腐镰刀菌烯醇的气相色谱分析[J].环境化学,1989,8(4):1-5.
[3]魏润蕴,王竹天.谷物中脱氧雪腐镰刀菌烯醇和雪腐镰刀菌烯醇的气相色谱测定[J].卫生研究,1996,25(4):242-245.
[4]黄志兵,游淑珠,邓舜洲,等.毛细管气相色谱法测定小麦和玉米中脱氧雪腐镰刀菌烯醇[J].食品科学,2007,28(4):241-245.
[5]唐吉旺,周丛,林源,等.毛细管-气相色谱法测定谷物中脱氧雪腐镰刀菌烯醇和雪腐镰刀菌烯醇的含量[J].理化检验-化学分册,2012,48(12):1441-1443.
[6]马立新.气相色谱仪测定进口小麦中镰刀菌毒素DON和NIV[J].中国国境卫生检疫杂志,1990,13(6):363-365.
[7]Tacke B K,Casper H H.Determination of Dexynivalenol in wheat,barley,and malt by column cleanup and gas chromatography with electron capture detection[J].Journal of AOAC international,1996,79(2):472-475.
[8]裴自友,韩航如,李亚浩,等.两种检测小麦中DON含量方法的比较与应用[J].麦类作物学报,2006,26(5):153-158.气质-液相
[9]ARIKA J,AIBERTO R,AND A.Analysis of the fusarium mycotetxius fusapmli&rin and trichothecenes in grai-ns using gas chromatography-mass spectrometry.[J]Ac Foos Chem,2004,52:1464-1469.气质
[10]隋凯,李军,卫锋.多功能净化-高效液相色谱法同时检测小麦中雪腐镰刀烯醇和脱氧雪腐镰刀烯醇[J].分析测试学报,2006,25(3):56-59.
[11]朱孟丽.高效液相色谱法对谷物汇总呕吐毒素的测定[J].粮食与饲料工业,2005,8:42-43.
[12]隋凯,李军,卫锋,等.谷物中脱氧雪腐镰刀菌烯醇的高效液相色谱检测及质谱确证[J].分析化学研究简报,2005,11(33):1643-1646.
[13]杨丹,耿志明,马鸿翔,等.高效液相色谱-紫外法同时检测小麦中DON、15ACDON和3ACDON[J].作物学报,2011,38(1):186-189.
[14]罗颖鹏,陈正行,王韧,等.固相萃取柱净化-高效液相色谱法测定小麦中脱氧雪腐镰刀菌烯醇[J].食品科学,2015,36(20):222-225.
[15]吴杰,陈万权,朱宝成.利用单克隆免疫亲和柱——高效液相色谱法检测小麦中DON毒素的研究[J].畜牧与饲料科学,2009,30(4):10-11.
[16]王伟,刘安法,李明奇,等.免疫亲和柱净化——高效液相色谱法检测小麦中脱氧雪腐镰刀菌烯醇[J].粮食与饲料工业,2013,1:60-61.
[17]欧阳毅,程树峰,唐芳,等.小麦脱氧雪腐镰刀菌烯醇(DON)检测方法的研究[J].粮油食品科技,2015,23(3):69-72.
[18]杨丹妮,汪海峰.小麦中呕吐毒素的ELISA和HPLC法检测[J].安徽农业科学,2013,41(3):1269-1270.
[19]龚燕,孙秀兰,邵景东.酶联免疫法检测呕吐毒素的方法研究[J].食品科学,2007,28(10):473-476.
[20]吴茂森,何晨阳.小麦赤霉病穗组织中黄色镰刀菌和DON毒素的定量分析[J].植物保护学报,2008,35(1):33-36.
[21]Usleber E,Erwin Martlbauer,Dietrich R,et al.Direct enzyme—linked immunosorbent assays for the detection of the 8-ketotriehothecene mycotoxins deoxynivalenol,3-acetyldeoxyivalenol,and 15-acetyldeoxyivalenol in buffer solutions.J Agric Food Chem,1991,39(11):2091-2095.
[22]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].北京: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,2016.
[23]Biselli S,Hummert C.Development of a multi-component method for Fusarium toxins using LC-MS/MSand its application during a survey for the content oft-2toxin and Dexynivalenol in various feed and food samples[J].Food additives&contaminants,2005,22(8):752-760.
[24]金海涛,张晓波,任红波,等.高效液相色谱质谱法快速测定小麦中DON、ZON、T-2的残留方法研究[J].粮食加工,2016,41(1):73-75.
[25]黄娟,陈国松,张晓燕,等.固相萃取-高效液相色谱-串联质谱法检测粮食及其制品中的呕吐毒素[J].色谱,2012,30(11):1203-1207.
[26]樊平声,沙国栋,张勇,等.南京市售小麦食品中DON毒素含量调查与风险评估[J].山地农业生物学报,2009,28(5):421-424.
[27]张祎,刘珊珊.江苏小麦生长期呕吐毒素监测预警研究进展[J].现代面粉工业,2016,1:21-22.
[28]白艺珍,李培武,丁小霞,等.我国粮油作物产品真菌毒素风险评估现状与对策研讨[J].农产品质量与安全,2015,5:54-58.
[29]张慧杰.小麦真菌毒素在加工过程中的消解、转移规律研究[D].北京,中国农业科学院,2014.