高效液相色谱-柱前衍生法测定食用油中黄曲霉毒素B_1和B_2的方法研究
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摘要
采用高效液相色谱-柱前衍生法对食用油中的黄曲霉毒素B1和B2进行检测。样品经85%乙腈水提取后,氮吹至近干,用正己烷和三氟乙酸衍生,在高效液相色谱仪荧光检测器上检测。结果表明:黄曲霉毒素B_1和B_2在0.2～40 ng·mL~(-1)内呈良好的线性关系,r> 0.999,黄曲霉毒素B_1和B_2添加浓度在0.2～10μg·kg~(-1),回收率范围为83.7%～92.8%,RSD为4.0%～8.3%,检出限分别为0.075μg·kg~(-1)和0.068μg·k~(-1),并用所建方法同GB 5009.22-2016中的第二法进行比较分析,从而为食用油中黄曲霉毒素B_1和B_2的检测提供一种更快速、更节约成本的方法。
A pre-column derivatization-high performance liquid chromatography method was developed for the simultaneous determination of aflatoxin B_1 and B_2 in edible oil. Samples were extracted with 85% acetoniltrile-water. The supernatant was concentrated by termovap sample concentrator, and derivated with hexane and trifluoroacetic acid. HPLC analysis was performed on a C18 column using fluorescence detection. The results showed good linearity in the range of 0.2 ～ 40 ng·mL~(-1), with correlation coefficients greater than 0.999. The limits of detection were 0.075 and0.068μg·kg~(-1) for aflatoxin B_1 and B_2 respectively. The recoveries were in the range of 83.7% ～ 92.8%, with the relative standard deviations from 4.0% to 8.3%. The method developed was convenient and cost-saving to be used effectively for determining aflatoxin B_1 and B_2 in edible oil.
A pre-column derivatization-high performance liquid chromatography method was developed for the simultaneous determination of aflatoxin B_1 and B_2 in edible oil. Samples were extracted with 85% acetoniltrile-water. The supernatant was concentrated by termovap sample concentrator, and derivated with hexane and trifluoroacetic acid. HPLC analysis was performed on a C18 column using fluorescence detection. The results showed good linearity in the range of 0.2 ～ 40 ng·mL~(-1), with correlation coefficients greater than 0.999. The limits of detection were 0.075 and0.068μg·kg~(-1) for aflatoxin B_1 and B_2 respectively. The recoveries were in the range of 83.7% ～ 92.8%, with the relative standard deviations from 4.0% to 8.3%. The method developed was convenient and cost-saving to be used effectively for determining aflatoxin B_1 and B_2 in edible oil.
引文
[1]居乃虎.黄曲霉毒素[M].北京:中国轻工业出版社,1980.
[2]Kensler T W,Roebuck B D,Wogan G N,et a1.Aflatoxin:A 50-year odyssey of mechanistic and translational toxicology[J].Toxicological Sciences,2011,120(1):28-48.
[3]Bressac B,Puisieux A,Kew M,et a1.p53mutation in hepatocellular carcinoma after anatoxin exposure[J].The Lancet.199l,338:1356-1359.
[4]国家卫生和计划生育委员会,国家食品药品监督管理总局.GB 2761-2017食品安全国家标准食品中真菌毒素限量[S].北京:中国标准出版社,2017.
[5]国家卫生和计划生育委员会,国家食品药品监督管理总局.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].北京:中国标准出版社,2016.
[2]Kensler T W,Roebuck B D,Wogan G N,et a1.Aflatoxin:A 50-year odyssey of mechanistic and translational toxicology[J].Toxicological Sciences,2011,120(1):28-48.
[3]Bressac B,Puisieux A,Kew M,et a1.p53mutation in hepatocellular carcinoma after anatoxin exposure[J].The Lancet.199l,338:1356-1359.
[4]国家卫生和计划生育委员会,国家食品药品监督管理总局.GB 2761-2017食品安全国家标准食品中真菌毒素限量[S].北京:中国标准出版社,2017.
[5]国家卫生和计划生育委员会,国家食品药品监督管理总局.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].北京:中国标准出版社,2016.