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免疫亲和柱净化和柱前衍生化后,用气相色谱-电子捕获检测法测定中药材及相关产品中的 T-2 和 HT-2 毒素的验证。

Validation of a gas chromatography-electron capture detection of T-2 and HT-2 toxins in Chinese herbal medicines and related products after immunoaffinity column clean-up and pre-column derivatization.

机构信息

Institute of Medicinal Plant Development, Chinese Academy of Medical Sciences, Peking Union Medical College, Beijing 100193, China.

Institute of Medicinal Plant Development, Chinese Academy of Medical Sciences, Peking Union Medical College, Beijing 100193, China; School of Pharmacy, Jiangsu University, Zhenjiang 212013, China.

出版信息

Food Chem. 2012 May 1;132(1):574-81. doi: 10.1016/j.foodchem.2011.10.073. Epub 2011 Oct 28.

DOI:10.1016/j.foodchem.2011.10.073
PMID:26434334
Abstract

A sensitive, reproducible and accurate gas chromatography-electron capture detection (GC-ECD) method was developed for simultaneous determination of T-2 and HT-2 toxins in Chinese herbal medicines (CHMs) and related products after immunoaffinity column (IAC) clean-up and pre-column derivatization with N-heptafluoro-butyryl imidazole (HFBI). Then, gas chromatography-spectrometry spectrometer (GC-MS) was applied to confirm the positive results and interfering peaks. The limits of detection (LODs) for T-2 and HT-2 toxins were 1.88 and 0.47ng/g, and the recoveries for different CHMs ranged from 89.2% to 99.1% with relative standard deviation (RSD) <6.0% for T-2 and from 85.9% to 99.0% with RSD <8.8% for HT-2 toxin, respectively. The validated method was successfully applied for the determination of T-2 and HT-2 toxins in 89 Chinese herbal medicines and 10 related products from various sources, where it was found that T-2 and HT-2 toxins were not detected in any of the tested samples. These results were reliable by confirmation using GC-MS. Some unknown peaks were interfering peaks not the target toxins.

摘要

建立了一种灵敏、重现性好、准确的免疫亲和柱净化-柱前衍生化结合气相色谱-电子捕获检测(GC-ECD)方法,用于同时测定中草药(CHM)及相关产品中的 T-2 和 HT-2 毒素。采用 N-七氟丁酰基-咪唑(HFBI)柱前衍生化,经免疫亲和柱(IAC)净化后,用气相色谱-质谱联用仪(GC-MS)对阳性结果和干扰峰进行确证。T-2 和 HT-2 毒素的检出限(LOD)分别为 1.88 和 0.47ng/g,不同 CHM 的回收率在 89.2%至 99.1%之间,相对标准偏差(RSD)<6.0%;HT-2 毒素的回收率在 85.9%至 99.0%之间,RSD<8.8%。该方法已成功应用于 89 种中草药和 10 种不同来源相关产品中 T-2 和 HT-2 毒素的测定,结果表明,所有测试样品均未检出 T-2 和 HT-2 毒素。GC-MS 确证结果可靠。一些未知峰为干扰峰,而非目标毒素。

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