液质联用同位素内标法同时测定3类小麦终产品中4种B类单端孢烯霉族类真菌毒素
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摘要
目的建立测定小麦终产品中4种B类单端孢烯霉族类真菌毒素的液质联用同位素内标法。方法馍馍、面包、面条3类样品粉碎混匀后经乙腈-水溶液(84∶16,V/V)提取,Romer Myco Sep 226多功能净化柱净化,Thermo TSQ Quantum Access Max三重四级杆质谱电喷雾负离子源(ESI-),多反应监测(MRM)方式进行检测,同位素内标法定量。结果 4种真菌毒素在5.00μg/L~500μg/L呈良好线性关系(r≥0.999 0),检出限为0.18μg/kg~0.25μg/kg,精密度相对标准偏差为2.46%~10.30%,加标回收率为70.8%~107.6%。结论此方法灵敏度高,线性范围较宽,可满足不同浓度的小麦终产品中4种真菌毒素的同时检测。
Objective To establish a method for the simultaneous determination of 4 kinds of type B trichothecene mycotoxins in wheat end products using high performance liquid chromatography-mass spectrometry( LC-MS/MS). Methods Three kinds of wheat flour products including steamed bun,bread and noodles were crushed and extracted with acetonitrile-water( 84∶16,V/V),then purified with Romer Myco Sep 226 column. The trichothecene mycotoxins were detected by UPLC-MS/MS system using negative electrospray ionization( ESI-) in multiple-reaction monitoring( MRM) mode,and quantified by the internal standard calibration curve of isotope dilution technique. Results 4 kinds of mycotoxins showed good linearity in the range of5. 00 μg/L-500 μg/L,with the correlation coefficients( r) ≥0. 999 0,the LODs of the mycotoxins ranged from 0. 18 μg/kg to0. 25 μg/kg. Meanwhile,the precision was within 2. 46%-10. 30%,and the average recovery was within 70. 8%-107. 6%.Conclusion The method was suitable for detecting 4 kinds of mycotoxins simultaneously in wheat end products at different concentrations with high accuracy,sensitivity and wide linear range.
Objective To establish a method for the simultaneous determination of 4 kinds of type B trichothecene mycotoxins in wheat end products using high performance liquid chromatography-mass spectrometry( LC-MS/MS). Methods Three kinds of wheat flour products including steamed bun,bread and noodles were crushed and extracted with acetonitrile-water( 84∶16,V/V),then purified with Romer Myco Sep 226 column. The trichothecene mycotoxins were detected by UPLC-MS/MS system using negative electrospray ionization( ESI-) in multiple-reaction monitoring( MRM) mode,and quantified by the internal standard calibration curve of isotope dilution technique. Results 4 kinds of mycotoxins showed good linearity in the range of5. 00 μg/L-500 μg/L,with the correlation coefficients( r) ≥0. 999 0,the LODs of the mycotoxins ranged from 0. 18 μg/kg to0. 25 μg/kg. Meanwhile,the precision was within 2. 46%-10. 30%,and the average recovery was within 70. 8%-107. 6%.Conclusion The method was suitable for detecting 4 kinds of mycotoxins simultaneously in wheat end products at different concentrations with high accuracy,sensitivity and wide linear range.
引文
[1]李慧芸,王军,张宝善.真菌毒素对食品的污染及防止措施[J].食品研究与开发,2004,25(3):26-30.
[2]张剑锋,孙艳芳,李健平,等.超高效液相色谱-质谱联用法同时测定食品中的B类单端孢烯霉族类真菌毒素[J].中国卫生检验杂志,2014,24(13):1856-1858.
[3]黄天培,何佩茹,潘洁茹,等.食品常见真菌毒素的危害及其防止措施[J].生物安全学报,2011,20(2):108-112.
[4]梁颖,张春辉,刘邻渭.气质联用测定DON和NIV及其衍生方法的比较研究[J].分析科学学报,2006,22(2):205-208.
[5]朱群英,索莉莉,胡美华.液质联用同位素内标法同时测定小麦粉中7种真菌毒素[J].现代预防医学,2014,41(23):4362-4377.
[6]张洁,伊艳杰,王金水,等.小麦赤霉病的防治技术研究进展[J].中国植保导刊,2014,34(1):24-28.
[7]郭建,王郑平,曹阳,等.高效液相色谱法测定粮食中的脱氧雪腐镰刀菌烯醇[J].粮食与食品工业,2014,21(6):87-93.
[8]林慧群.小麦赤霉病粒与脱氧雪腐镰刀烯醇、玉米赤霉烯酮关系的研究[J].粮食与食品工业,2014,21(4):128-130.
[9]庞炜,王治伦,吕社民,等.真菌毒素DON研究进展[J].中国地方病防治杂志,1996,11(6):349-351.
[10]Zhang XH,Xie TX,Li SS,et al.Contamination of fungi and mycotoxins in foodstuffs in high risk area of esophageal cancer[J].Biomed Environ Sci,1998,11(2):140-146.
[11]Pronyk C,Cenkowski S,Abramson D.Superheated steam reduction of deoxynivalenol in naturally contaminated wheat kernels[J].Food Control,2006,17(10):789-796.
[12]杨大进,李宁.2015年国家食品污染和有害因素风险工作手册[M].北京:中国标准出版社,2015:422-428.
[13]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,2014,40(4):691-701.
[14]Zhang XH,Xie TX,Li SS,et al.Contamination of fungi and mycotoxins in foodstuffs in high risk area of esophageal cancer[J].Biomed Environ Sci,1998,11(2):140-146.
[15]张帆,吴志远,吴健丽,等.食管癌高发区粮食中镰刀菌毒素的含量及其致突变作用[J].中华预防医学杂志,2000,34(1):53.
[16]王文龙,刘阳,李少英,等.脱氧学雪腐镰刀烯醇与人类健康[J].食品研究与开发,2008,29(6):153-157.
[2]张剑锋,孙艳芳,李健平,等.超高效液相色谱-质谱联用法同时测定食品中的B类单端孢烯霉族类真菌毒素[J].中国卫生检验杂志,2014,24(13):1856-1858.
[3]黄天培,何佩茹,潘洁茹,等.食品常见真菌毒素的危害及其防止措施[J].生物安全学报,2011,20(2):108-112.
[4]梁颖,张春辉,刘邻渭.气质联用测定DON和NIV及其衍生方法的比较研究[J].分析科学学报,2006,22(2):205-208.
[5]朱群英,索莉莉,胡美华.液质联用同位素内标法同时测定小麦粉中7种真菌毒素[J].现代预防医学,2014,41(23):4362-4377.
[6]张洁,伊艳杰,王金水,等.小麦赤霉病的防治技术研究进展[J].中国植保导刊,2014,34(1):24-28.
[7]郭建,王郑平,曹阳,等.高效液相色谱法测定粮食中的脱氧雪腐镰刀菌烯醇[J].粮食与食品工业,2014,21(6):87-93.
[8]林慧群.小麦赤霉病粒与脱氧雪腐镰刀烯醇、玉米赤霉烯酮关系的研究[J].粮食与食品工业,2014,21(4):128-130.
[9]庞炜,王治伦,吕社民,等.真菌毒素DON研究进展[J].中国地方病防治杂志,1996,11(6):349-351.
[10]Zhang XH,Xie TX,Li SS,et al.Contamination of fungi and mycotoxins in foodstuffs in high risk area of esophageal cancer[J].Biomed Environ Sci,1998,11(2):140-146.
[11]Pronyk C,Cenkowski S,Abramson D.Superheated steam reduction of deoxynivalenol in naturally contaminated wheat kernels[J].Food Control,2006,17(10):789-796.
[12]杨大进,李宁.2015年国家食品污染和有害因素风险工作手册[M].北京:中国标准出版社,2015:422-428.
[13]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,2014,40(4):691-701.
[14]Zhang XH,Xie TX,Li SS,et al.Contamination of fungi and mycotoxins in foodstuffs in high risk area of esophageal cancer[J].Biomed Environ Sci,1998,11(2):140-146.
[15]张帆,吴志远,吴健丽,等.食管癌高发区粮食中镰刀菌毒素的含量及其致突变作用[J].中华预防医学杂志,2000,34(1):53.
[16]王文龙,刘阳,李少英,等.脱氧学雪腐镰刀烯醇与人类健康[J].食品研究与开发,2008,29(6):153-157.