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通过测定何首乌中多种真菌毒素的含量,探讨其致肝毒性原因。采用高效液相色谱-串联质谱法检测何首乌中黄曲霉毒素B1,B2,G1,G2,赭曲霉毒素A,B,T-2毒素,HT-2毒素,伏马毒素B1,B2,玉米赤霉烯酮和脱氧雪腐镰刀菌烯醇共12种真菌毒素的含量。样品采用改良的Qu ECh ERS方法提取,使用Welch Ultimate XBC18色谱柱(4.6 mm×100 mm,2.5μm)分离,甲醇-含0.1%乙酸的2 mmol·L~(-1)醋酸铵水溶液为流动相梯度洗脱,多反应监测模式下测定,外标法定量。结果表明,12种真菌毒素在0.1~200μg·kg~(-1)线性关系良好,相关系数为0.996 3~0.999 9,加标回收率为71.19%~98.68%,相对标准偏差为1.7%~13%。该方法操作简单、准确、灵敏,可用于何首乌中多种真菌毒素的快速测定。结果显示,41批样品中的15批检出了真菌毒素,涉及毒素类型有AFB1,AFG2,FB1,OTB,T-2,HT-2,FB2和OTA共8种,毒素在0.51~1 643.2μg·kg~(-1)。其中1批制首乌中检测到AFB1,达6.8μg·kg~(-1),超出了其在2015年版《中国药典》中的限量标准(5μg·kg~(-1))。AFB1具有明确的肝毒性。因此,推测何首乌在产地加工、储存运输过程中产生的少量霉变样品是其导致肝损伤的重要因素之一。
By determining the content of various mycotoxins in Polygonum multiflorum, the cause of hepatotoxicity was explored. The contents of aflatoxin B1, B2, G1, G2, ochratoxin A, B, T-2 toxin, HT-2 toxin, fumonisins B1, B2, Enkephalin and deoxynivalenol a total of 12 kinds of mycotoxin content. Samples were extracted using a modified QuECh ERS method and separated on a Welch Ultimate XBC18 column (4.6 mm × 100 mm, 2.5 μm). Methanol - a 2 mmol·L -1 ammonium acetate aqueous solution containing 0.1% acetic acid as a mobile phase Gradient elution, multi-reaction monitoring mode determination, external standard quantitative. The results showed that the linear relationship between 12 mycotoxins and 0.1 ~ 200 μg · kg -1 was good, the correlation coefficient was 0.996 3 ~ 0.999 9, the recoveries were 71.19% ~ 98.68% and the relative standard deviations were 1.7% ~ 13 %. The method is simple, accurate and sensitive and can be used for the rapid determination of various mycotoxins in Polygonum multiflorum. The results showed that mycotoxins were detected in 15 batches of 41 batches of samples and 8 types of toxins including AFB1, AFG2, FB1, OTB, T-2, HT-2, FB2 and OTA were found. Toxins ranged from 0.51 to 1643.2 μg · Kg ~ (-1). Among them, AFB1 was detected in one batch of Radix Polygalae, up to 6.8 μg · kg -1, which exceeded the limit of 5 μg · kg -1 in the Chinese Pharmacopoeia 2015 edition. AFB1 has definite hepatotoxicity. Therefore, it is speculated that Polygonum multiflorum in the processing, storage and transportation of small amounts of mildew samples is one of the important factors that lead to liver damage.