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QuEChERS提取-高效液相色谱法测定泰山虫草中4种黄曲霉毒素的含量 被引量:7

Determination of 4 Aflatoxins in Cordyceps Taishanensis by High Performance Liquid Chromatography with QuEChERS Extraction
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摘要 取泰山虫草样品2.50g,加入7.5mL水和含0.1%(体积分数)乙酸的乙腈混合溶液10mL,涡旋振荡1min,再加入无水硫酸镁4.0g和氯化钠1.0g,离心,取上清液1.0 mL于含150mg无水硫酸镁、50mg N-丙基乙二胺、50mg C18填料、12mg石墨化碳黑的2mL分散固相萃取管中,涡旋振荡30s,取上清液经过0.22μm有机滤膜进行过滤,采用高效液相色谱法测定其中4种黄曲霉毒素的含量。结果表明:4种黄曲霉毒素的质量浓度在一定范围内与其峰面积之间呈线性关系,检出限(3S/N)在0.06~0.20μg·kg-1之间。按照标准加入法进行加标回收试验,测得回收率在92.4%~102%之间,测定值的相对标准偏差(n=6)在2.7%~3.5%之间。 An aliquot(2.50 g)of the cordyceps taishanensis was taken and 7.5 mL of water and 10 mL of acetonitrile solution containing 0.1%(φ)acetic acid were added.The mixture was shaken vortically for 1 min,and then 4.0 g of anhydrous magnesium sulfate and 1.0 g of sodium chloride were added.After centrifugation,1.0 mL of the supernatant was taken in the disperse solid phase extraction tube(2 mL,containing 150 mg of anhydrous magnesium sulfate,50 mg N-propyl ethylenediamine,50 mg of C18 filler and 12 mg of graphitized carbon black).The mixture was shaken vortically for 30 s.The supernatant was filtered through 0.22μm organic filter membrane,and the contents of 4 aflatoxins were determined by high performance liquid chromatography.As shown by the results,linear relationships between values of peak area and mass concentration of 4 aflatoxins were found in definite ranges,with detection limits(3 S/N)in the range of 0.06-0.20μg·kg^-1.Test for recovery was made by standard addition method,giving results in the range of 92.4%-102%,and RSDs(n=6)were found in the range of2.7%-3.5%.
作者 叶雪玲 陈小燕 姜小涵 赵凤春 李艳玲 田园 YE Xueling;CHEN Xiaoyan;JIANG Xiaohan;ZHAO Fengchun;LI Yanling;TIAN Yuan(Shandong Provincial Key Laboratory of Traditional Chinese Medicine Biotechnology College of Life Sciences,Taishan Medical University,Tai'an 271016,China;Shandong Provincial Key Laboratory of Agricultural Microbiology,College of Life Sciences,Shandong Agricultural University,Tai'an 271018,China)
出处 《理化检验(化学分册)》 CAS CSCD 北大核心 2019年第4期442-446,共5页 Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
基金 国家自然科学基金项目(21602152) 山东省自然科学基金项目(ZR2016BB01) 泰安市科技发展计划项目(2016NS1214) 国家级大学生创新创业训练计划项目(201710439309) 山东省农业微生物重点实验室开放课题基金(SDKL2017015)
关键词 高效液相色谱法 QUECHERS 黄曲霉毒素 泰山虫草 high performance liquid chromatography QuEChERS aflatoxin cordyceps taishanensis
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