超高压液相色谱-串联质谱法测定粮食中多种真菌毒素残留
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摘要
建立了使用超高压液相色谱串联质谱法测定粮食中多种真菌毒素含量的分析方法。样品通过乙腈-水(80∶20,V∶V)混合液提取,超声提取20 min,离心后取上清液,用正己烷去脂后,用Oasis PRi ME HLB固相萃取柱净化,通过RRHD SB-C_(18)型色谱柱分离,在正离子及负离子多反应监测模式下分析定量。结果表明,多种真菌毒素在0.1～10 ng/mL,5～500 ng/mL的质量浓度范围内线性良好,空白样品加标的回收率为73.4%～108.9%,相对标准偏差均小于10%。该方法快速、准确,可同时测定粮食中真菌毒素含量。
An analysis method is established for detecting the content of mycotoxins in cereals using ultra high performance liquid chromatographic tandem mass spectromrtry.The sample was extracted with acetonitrile-water(80 ∶20,V∶V)mixture,ultrasonically extracted for 20 min,centrifuged,and the supernatant was removed.The supernatant was degreased with n-hexane,and purified by Oasis PRi ME HLB solid phase column.And analyzed in positive and negative MRM mode after separated by RRHD SB-C_(18) column.The results showed that a good linearity in the range of 0.1～10 ng/m L and 5～500 ng/mL.The recovery at different concentration levels of mycotoxins in blank showed values in range of 73.4% ～108.9%,with RSD less than 10%.The method had the characteristics of high sensitive and specific,simultaneous determination of mycotoxins in cereals.
An analysis method is established for detecting the content of mycotoxins in cereals using ultra high performance liquid chromatographic tandem mass spectromrtry.The sample was extracted with acetonitrile-water(80 ∶20,V∶V)mixture,ultrasonically extracted for 20 min,centrifuged,and the supernatant was removed.The supernatant was degreased with n-hexane,and purified by Oasis PRi ME HLB solid phase column.And analyzed in positive and negative MRM mode after separated by RRHD SB-C_(18) column.The results showed that a good linearity in the range of 0.1～10 ng/m L and 5～500 ng/mL.The recovery at different concentration levels of mycotoxins in blank showed values in range of 73.4% ～108.9%,with RSD less than 10%.The method had the characteristics of high sensitive and specific,simultaneous determination of mycotoxins in cereals.
引文
[1]吴永宁,李筱薇.第四次中国总膳食研究[M].北京:化学工业出版社,2015:253-260.
[2]李萌萌,关二旗,卞科,等.真菌毒素的辐照降解及产物解析研究进展[J].粮食与饲料工业,2013(1):14-18.
[3]傅勇,曹纪亮,杨小丽,等.真菌毒素检测的前处理技术及其应用[J].中国卫生检验杂志,2012(6):1 462-1466.
[4]卢安根,莫建光,杜寒春,等.酶联免疫法快速检测牛奶及其制品中的黄曲霉毒素B1[J].广西科学院学报,2010,26(3):306-308.
[5]廉慧锋,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种真菌毒素[J].食品科学,2010,31(20):360-366.
[6]辛媛媛,张艳,王松雪,等.UPLC-MS/MS法测定玉米中13种真菌毒素[J].中国粮油学报,2015(12):126-130.
[2]李萌萌,关二旗,卞科,等.真菌毒素的辐照降解及产物解析研究进展[J].粮食与饲料工业,2013(1):14-18.
[3]傅勇,曹纪亮,杨小丽,等.真菌毒素检测的前处理技术及其应用[J].中国卫生检验杂志,2012(6):1 462-1466.
[4]卢安根,莫建光,杜寒春,等.酶联免疫法快速检测牛奶及其制品中的黄曲霉毒素B1[J].广西科学院学报,2010,26(3):306-308.
[5]廉慧锋,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种真菌毒素[J].食品科学,2010,31(20):360-366.
[6]辛媛媛,张艳,王松雪,等.UPLC-MS/MS法测定玉米中13种真菌毒素[J].中国粮油学报,2015(12):126-130.