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免疫亲和柱净化-在线柱后光化学衍生HPLC-FLD检测莲子中黄曲霉毒素B_1,B_2,G_1,G_2及其液质确证 被引量:33

Determination of aflatoxins in Nelumbinis Semen by immunoaffinity column clean-up and HPLC-FLD with on-line post-column photochemical derivatization and LC-MS/MS confirmation
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摘要 目的:建立高效液相色谱-在线柱后光化学衍生-荧光检测器检测药食同源中药材莲子中黄曲霉毒素B1,B2,G1,G2的含量,并采用液质联用法进行确证。方法:样品以甲醇-水(80∶20)溶液提取,经免疫亲和柱净化后,利用在线柱后光化学衍生-HPLC-FLD进行分析测定。并进一步采用LC-MS/MS对阳性样品进行确证。结果:在优化条件下,黄曲霉毒素B1,G1在0.3~30μg.L-1,黄曲霉毒素B2,G2在0.09~9.0μg.L-1线性关系良好,r>0.999 9,回收率86.7%~99.1%,RSD<4.87%。黄曲霉毒素B1,B2,G1,G2的检测限(LOD)分别为0.08,0.03,0.10,0.03μg.kg-1。所测的20批莲子样品中,有14批样品的黄曲霉毒素检测结果呈阳性,其中黄曲霉毒素B1的污染水平为0.40~586μg.kg-1,黄曲霉毒素总量(B1+B2+G1+G2)的污染水平为0.40~602.5μg.kg-1。通过LC-MS/MS确证,在与对照品相同的保留时间处,样品与对照品有相同的特征离子碎片,排除了样品假阳性的可能。结论:该方法简便快速,灵敏度高,重复性好,适用于莲子中黄曲霉毒素的检测。 To determine the contents of aflatoxin B1, B2, G1 and G2 in Nelumbinis Semen using on-line post-column photo- chemical derivatization-HPLC-FLD method and verify the method by LC-MS method. Method: The samples were extracted with MeOH-H20 (80: 20) and purified with inmunoaffinity column, aflatoxins were analyzed by HPLC-FLD with post-column photochemical derivatizaton. The positive samples were further confirmed by LC-MS/MS. Result: On optimum conditions, aflatoxin B1, G1 ranging 0. 3-30 mg·L-1 showed a good linear relationship with aflatoxin B2 , G2 ranging 0. 09-9. 0 mg ·L- 1 with r 〉 0. 999 9. The recoveries ranged between 86. 7% and 99. 1% , with RSDs all bellow 4. 87%. LOD of aflatoxin B1 , B2 , GI and G: were 0. 08, 0. 03, 0. 10, 0. 03 μg·kg^-1 , respectively. Among 20 Nelumbinis Semen samples, 14 were found to contain aflatoxin B1 ranging from 0. 40 to 586μg·kg^-1. The total content of aflatoxin B1 , B2 , G1 and G2 were between 0. 40 and 602. 5μg·kg^-1. By LC-MS/MS method, the same fragment ions were founded in samples and the control group at the same retention times, ruling out the possibility of false positive samples. Conclusion: The method is simple, highly sensitive and reproducible for the determination of aflatoxins in Nelumbinis SeInOFI.
出处 《中国中药杂志》 CAS CSCD 北大核心 2012年第3期305-309,共5页 China Journal of Chinese Materia Medica
基金 国家"重大新药创制"科技重大专项(2009ZX09502-025 2010ZX09301-002-001) 国家中医药管理局中医药行业科研专项(200807042)
关键词 黄曲霉毒素 莲子 在线光化学衍生 高效液相色谱 液质确证 aflatoxins Nelumbinis Semen on-line photochenaical derivatization HPLC LC-MS/MS
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