Detenuination of 14 mycotoxins in Chinese herbs by liquid chromatography-tandem mass spectrometry with immunoaffinity purification
Detenuination of 14 mycotoxins in Chinese herbs by liquid chromatography-tandem mass spectrometry with immunoaffinity purification
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DOI：
10.3724/sp.j.1123.2011.00495
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发表时间：
2011-06-01
影响因子：
0.7
通讯作者：
Mi Jiebo
中科院分区：
文献类型：
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作者：
Ge Baokun;Zhao Kongxiang;Mi Jiebo
建立了中草药中黄曲霉毒素、T-2、HT-2、伏马菌素、赭曲霉毒素A、玉米赤霉烯酮等14种真菌毒素的液相色谱-串联四极杆质谱（LC-MS/MS）测定方法。样品依次用磷酸盐缓冲液（PBS）和甲醇提取，经高选择性多功能免疫亲和柱纯化。用PBS（含0.1%Twain）和水洗涤柱，然后用甲醇洗脱。将沉淀物在氮气下干燥，溶于甲醇-10 mmol/L NH 4Ac（40：60，v/v）溶液中。霉菌毒素在沃茨Xterra C18 MS柱（100 mm x 2.1 mm，3.5 μ m）上分离，并通过MS/MS检测。14种霉菌毒素的定量限（LOQ）为1.0 - 5.0 μ g/kg。在1.0、5.0、10.0 μ g/kg 3个添加水平下，14种真菌毒素的平均回收率为71.9%~ 99.7%，相对标准偏差（RSD，n = 6）为4.8%~ 15.8%。该方法快速、灵敏、准确，适用于中药中14种真菌毒素的测定。黄曲霉毒素的定量限符合国内外要求。
A method was developed for the determination of 14 mycotoxins, aflatoxins, T-2, HT-2, fumonisins, ochratoxin A, zearalenone, etc. in Chinese herbs by liquid chromatography-tandem quadrupole mass spectrometry (LC-MS/MS). The sample was extracted with phosphate buffer solution (PBS) and methanol in turn, and then purified by a high selective multi-functional immunoaffinity column. The column was washed by PBS (containing 0.1% Twain) and water, and then eluted by methanol. The eluate was dried under nitrogen, dissolved in methanol-10 mmol/L NH4Ac (40 : 60, v/v) solution. The mycotoxins were separated on a Waters Xterra C18 MS column (100 mm x 2.1 mm, 3.5 mu m) and detected by MS/MS. The limits of quantification (LOQs) of the 14 mycotoxins were from 1.0 to 5.0 mu g/kg. The average recoveries of the 14 mycotoxins spiked in Chinese herbs (Ginseng, Campanulaceae, Radix and Ophiopogonis) ranged from 71.9% to 99.7% at the three spiked levels of 1.0, 5.0, 10.0 mu g/kg, and the relative standard deviations (RSDs, n = 6) were between 4.8% and 15.8%. The method is rapid, sensitive and accurate, and suitable for the determination of the 14 mycotoxins in Chinese medicines. The quantification limits of aflatoxins can meet the domestic and foreign requirements.