摘要
目的建立复合免疫亲和柱净化-超高效液相色谱-串联质谱法测定婴幼儿谷物辅食中10种真菌毒素的方法。方法样品经乙腈-水-甲酸(80+19+1,V/V/V)提取,真菌毒素六合一免疫亲和柱净化。色谱柱采用Waters HSS T3柱(2.1 mm×100 mm,1.8μm),流动相为乙腈-0.1%甲酸溶液(ESI+),乙腈-0.1%氨水溶液(ESI-),梯度洗脱;质谱采用电喷雾离子源,多反应监测模式进行检测,同位素内标法定量。结果 10种真菌毒素在一定范围内线性关系良好(r>0.99);检测限(LOD)和定量限(LOQ)分别为0.05μg/kg^15μg/kg和0.15μg/kg^45μg/kg;低、中、高3个浓度的相对回收率分别为94.6%~106.3%、95.0%~108.1%、88.9%~115.6%,精密度(RSD)分别为4.2%~11.3%、2.3%~13.7%、2.4%~9.4%。结论该方法灵敏、准确、稳定,适用于婴幼儿谷物辅食中真菌毒素多组分的测定。
Objective A method was developed for the determination of 10 mycotoxins in cereal-based complementary foods for infants and young children by ultra high performance liquid chromatography coupled to mass spectrometry using composite immunoaffinity column clean-up. Methods The samples were extracted by acetonitrile-H2 O-formic acid（80 ＋ 19 ＋ 1,V/V/V） and purified by composite immunoaffinity column,and then analyzed by LC-MS/MS. The chromatographic column was Waters HSS T3 column（2. 1 mm × 100 mm,1. 8 μm）,and the flowing phase was comprised with acetonitrile-0. 1% formic acid solution（ESI＋） or acetonitrile-0. 1% ammonia solution（ESI-） with gradient eluting; the mass spectrometry was run with electrospray ion source and multiple reaction monitoring mode for determination. Results 10 mycotoxins showed good linear correlations in the specified linear range（r 〉 0. 99）. Limit of detection（LOD） and limit of quantitation（LOQ） were within0. 05 μg/kg-15 μg/kg and 0. 15 μg/kg-45 μg/kg,respectively. The recoveries of low,medium and high concentration were within 94. 6%-106. 3%,95. 0%-108. 1% and 88. 9%-115. 6%,respetively; RSD was within 4. 2%-11. 3%,2. 3%-13. 7% and 2. 4%-9. 4%,respetively. Conclusion The proposed method was sensitive,accurate and stable,which could meet the monitoring requirements of multi-component mycotoxins in cereal-based complementary foods for infants and young children.
作者
和佳鸳
张春玲
蒲彦利
王洪波
戴莉人
徐虹
HE Jia - yuan, ZHANG Chun - ling, PU Yan- li, WANG Hong - bo, DAI Li - ren, XU Hong(Zhenjiang Center for Disease Control and Prevention, Zhenjiang, Jiangsu 212000, Chin)
出处
《中国卫生检验杂志》
CAS
2018年第9期1044-1048,共5页
Chinese Journal of Health Laboratory Technology
关键词
复合免疫亲和柱净化-超高效液相色谱-串联质谱法
婴幼儿谷物辅食
真菌毒素
Composite immunoaffinity column cleanup-ultra-performance liquid chromatography-tandem mass spectrometry
Cereal-based complementary foods
Mycotoxins
