光化学柱后衍生–高效液相色谱法测定婴幼儿营养米粉中的黄曲霉毒素B1
|
摘要
建立婴幼儿营养米粉中黄曲霉毒素B1的高效液相色谱荧光检测器测定方法。样品以甲醇–水(体积比70∶30)溶液匀质提取,过黄曲霉毒素B1免疫层析亲和柱净化,经CNW Athena C18色谱柱分离和光化学柱后衍生反应器衍生后,用带有荧光检测器的高效液相色谱仪测定。采用峰面积外标法定量黄曲霉毒素B1含量。黄曲霉毒素B1在0～10μg/L的浓度范围内线性关系良好,相关系数为0.999 8,检出限为0.25μg/kg。在3个添加水平下加标回收率为97.7%～106.9%,测定结果的相对标准偏差为1.7%(n=6)。该方法的灵敏度、准确度、精密度均符合黄曲霉毒素B1的检测技术要求,适用于婴幼儿营养米粉中黄曲霉毒素B1的日常检测。
A high performance liquid chromatography(HPLC) coupled with post–column photochemical derivatization method was developed for the determination of aflatoxin B1 in rice cereal for infants and young children. The sample was extracted with methanol–water(volume ratio was 70∶30) then purified by immunoaffinity column for the purification aflatoxin B1. The high performance liquid chromatography(HPLC) separation was performed on a CNW Athena C18 column with methanol and water. The aflatoxin B1 was determined by fluorescence detection(FLD) after photochemical derivatization,and quantified by the peak area external standard method. The calibration curve showed good linearity in 0–10 μg/L range with correlation coefficient of 0.999 8. The limit of detection(LOD) was 0.25 μg/kg for aflatoxin B1 in rice cereal for infants and young children. The recovery of aflatoxin B1 spiked at there levels in rice cereal for infants and young children ranged from 97.7% to 106.9% with the relative standard deviation(RSD) of 1.7%(n=6). The sensitivity,accuracy and precision of the method can meet the technical standards requirement of the aflatoxin B1 determination. Therefore the method can be applied to the determination of the aflatoxin B1 in rice cereal for infants and young children.
A high performance liquid chromatography(HPLC) coupled with post–column photochemical derivatization method was developed for the determination of aflatoxin B1 in rice cereal for infants and young children. The sample was extracted with methanol–water(volume ratio was 70∶30) then purified by immunoaffinity column for the purification aflatoxin B1. The high performance liquid chromatography(HPLC) separation was performed on a CNW Athena C18 column with methanol and water. The aflatoxin B1 was determined by fluorescence detection(FLD) after photochemical derivatization,and quantified by the peak area external standard method. The calibration curve showed good linearity in 0–10 μg/L range with correlation coefficient of 0.999 8. The limit of detection(LOD) was 0.25 μg/kg for aflatoxin B1 in rice cereal for infants and young children. The recovery of aflatoxin B1 spiked at there levels in rice cereal for infants and young children ranged from 97.7% to 106.9% with the relative standard deviation(RSD) of 1.7%(n=6). The sensitivity,accuracy and precision of the method can meet the technical standards requirement of the aflatoxin B1 determination. Therefore the method can be applied to the determination of the aflatoxin B1 in rice cereal for infants and young children.
引文
[1]Deiner U L,Cole R J,Sanders T H,et al.Epidemiology of aflatoxin formation by Aspergillus flavus[J].Annu RevPhytopathol,1987,25:249–270.
[2]Kurtzman C P,Horn B W,Hesseltine C W.Aspergillus nomius,a new aflatoxin producing species related to Aspergillus flavus and Aspergillus tamari[J].Antoine van Leeuwenhoek,1987,53:147–158.
[3]Cotty P J,Bhatnagar D.Variability among atoxigenic Aspergillus flavus strains in ability to prevent aflatoxin contamination and production of aflatoxin biosynthetic pathway enzymes[J].Appl Environ Microbiol,1994,60:2 248–2 251.
[4]Chang H L,Devries J W.Rapid high pressure liquid chromagraphic determination of aflatoxin M1 in milk and nonfat dry milk[J].Journal of Association Official Analysis Chemistry,1982,66(4):913–917.
[5]马志科,昝林森.黄曲霉毒素危害、检测方法及生物降解研究进展[J].动物医学进展,2009,30(9):91–94.
[6]范蓓,李庆鹏,哈益明.关注黄曲霉毒素国内外限量标准,完善食品安全保障措施[J].食品工业科技,2010(12):26–27.
[7]潘崴,庞广昌,张昀.黄曲霉毒素与食品安全[J].食品研究与开发,2004,25(6):11–13.
[8]李书国,陈辉,李雪梅,等.粮油食品中黄曲霉毒素检测方法综述[J].粮油食品科技,2009,17(2):62–65.
[9]Iarc W.Some naturally occurring substances:food items and constituents,heterocyclic aromatic amines,and myeotoxirts[J].IARC Monographs on the Evaluation of Carcinogenic Risk to humans,1993,56:245–362.
[10]Elisabete Y S,mario A,Fabia Y,et al.Evaluation of fumonisinaflatoxin co-occurrence in Brazilian corn hybrids by ELISA[J].Food Addit Contam,2001,18(8):719–729.
[11]GB 2761–2011食品安全国家标准食品中真菌毒素限量[S].
[12]GB 5009.24–2010食品安全国家标准食品中黄曲霉毒素M1和B1的测定[S].
[13]张宸,岳田利,高振鹏,等.食品中黄曲霉毒素B1检测方法研究进展[J].农产品加工·学刊,2008(7):18–21.
[14]谢刚,王松雪,张艳.超高效液相色谱法快速检测粮食中黄曲霉毒素的含量[J].分析化学,2013,41(2):223–228.
[15]刘坚,余敦年,熊宁,等.高效液相色谱法对稻谷及稻谷籽粒中黄曲霉毒素的测定研究[J].中国粮油学报,2011,26(4):107–110.
[16]姜兆兴,曹旭,李智瑾.高效液相色谱法测定粮谷中黄曲霉毒素B1的研究[J].粮食与食品工业,2005,12(6):61–63.
[17]罗建波,谭小秋.高效液相色谱法测定婴幼儿食品中的黄曲霉毒素B1[J].广东卫生防疫,1992,18(2):52–55.
[18]丁轶聪,王桂苓,张伟伟.荧光色谱–柱后光化学衍生法测定食品中的黄曲霉毒素B1[J].化学分析计量,2013,22(6):56–58.
[19]Gobel R,Lusky K.Simultaneous determination of aflatoxins,ochratox in A,and zearalenone in grains by new immunoaffinity column/liquid chromatography[J].Journal of AOAC International,2004(2):411–415.
[20]GB/T 27404–2008实验室质量控制规范食品理化检测[S].
[2]Kurtzman C P,Horn B W,Hesseltine C W.Aspergillus nomius,a new aflatoxin producing species related to Aspergillus flavus and Aspergillus tamari[J].Antoine van Leeuwenhoek,1987,53:147–158.
[3]Cotty P J,Bhatnagar D.Variability among atoxigenic Aspergillus flavus strains in ability to prevent aflatoxin contamination and production of aflatoxin biosynthetic pathway enzymes[J].Appl Environ Microbiol,1994,60:2 248–2 251.
[4]Chang H L,Devries J W.Rapid high pressure liquid chromagraphic determination of aflatoxin M1 in milk and nonfat dry milk[J].Journal of Association Official Analysis Chemistry,1982,66(4):913–917.
[5]马志科,昝林森.黄曲霉毒素危害、检测方法及生物降解研究进展[J].动物医学进展,2009,30(9):91–94.
[6]范蓓,李庆鹏,哈益明.关注黄曲霉毒素国内外限量标准,完善食品安全保障措施[J].食品工业科技,2010(12):26–27.
[7]潘崴,庞广昌,张昀.黄曲霉毒素与食品安全[J].食品研究与开发,2004,25(6):11–13.
[8]李书国,陈辉,李雪梅,等.粮油食品中黄曲霉毒素检测方法综述[J].粮油食品科技,2009,17(2):62–65.
[9]Iarc W.Some naturally occurring substances:food items and constituents,heterocyclic aromatic amines,and myeotoxirts[J].IARC Monographs on the Evaluation of Carcinogenic Risk to humans,1993,56:245–362.
[10]Elisabete Y S,mario A,Fabia Y,et al.Evaluation of fumonisinaflatoxin co-occurrence in Brazilian corn hybrids by ELISA[J].Food Addit Contam,2001,18(8):719–729.
[11]GB 2761–2011食品安全国家标准食品中真菌毒素限量[S].
[12]GB 5009.24–2010食品安全国家标准食品中黄曲霉毒素M1和B1的测定[S].
[13]张宸,岳田利,高振鹏,等.食品中黄曲霉毒素B1检测方法研究进展[J].农产品加工·学刊,2008(7):18–21.
[14]谢刚,王松雪,张艳.超高效液相色谱法快速检测粮食中黄曲霉毒素的含量[J].分析化学,2013,41(2):223–228.
[15]刘坚,余敦年,熊宁,等.高效液相色谱法对稻谷及稻谷籽粒中黄曲霉毒素的测定研究[J].中国粮油学报,2011,26(4):107–110.
[16]姜兆兴,曹旭,李智瑾.高效液相色谱法测定粮谷中黄曲霉毒素B1的研究[J].粮食与食品工业,2005,12(6):61–63.
[17]罗建波,谭小秋.高效液相色谱法测定婴幼儿食品中的黄曲霉毒素B1[J].广东卫生防疫,1992,18(2):52–55.
[18]丁轶聪,王桂苓,张伟伟.荧光色谱–柱后光化学衍生法测定食品中的黄曲霉毒素B1[J].化学分析计量,2013,22(6):56–58.
[19]Gobel R,Lusky K.Simultaneous determination of aflatoxins,ochratox in A,and zearalenone in grains by new immunoaffinity column/liquid chromatography[J].Journal of AOAC International,2004(2):411–415.
[20]GB/T 27404–2008实验室质量控制规范食品理化检测[S].
© 2004-2018 中国地质图书馆版权所有 京ICP备05064691号 京公网安备11010802017129号 地址：北京市海淀区学院路29号 邮编：100083 电话：办公室：(+86 10)66554848；文献借阅、咨询服务、科技查新：66554700 |