Determination of 4 Aflatoxins in Cordyceps Taishanensis by High Performance Liquid Chromatography with QuEChERS Extraction
摘 要
取泰山虫草样品2.50 g,加入7.5 mL水和含0.1%(体积分数)乙酸的乙腈混合溶液10 mL,涡旋振荡1 min,再加入无水硫酸镁4.0 g和氯化钠1.0 g,离心,取上清液1.0 mL于含150 mg无水硫酸镁、50 mg N-丙基乙二胺、50 mg C18填料、12 mg石墨化碳黑的2 mL分散固相萃取管中,涡旋振荡30 s,取上清液经过0.22 μm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0.06~0.20 μg·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。
Abstract
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 0.22 μm 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 (3S/N) in the range of 0.06-0.20 μg·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 of 2.7%-3.5%.
中图分类号 O657.7 DOI 10.11973/lhjy-hx201904013
所属栏目 工作简报
基金项目 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)
收稿日期 2018/7/16
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备注叶雪玲,本科,研究方向为生物技术
引用该论文: YE Xueling,CHEN Xiaoyan,JIANG Xiaohan,ZHAO Fengchun,LI Yanling,TIAN Yuan. Determination of 4 Aflatoxins in Cordyceps Taishanensis by High Performance Liquid Chromatography with QuEChERS Extraction[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2019, 55(4): 442~446
叶雪玲,陈小燕,姜小涵,赵凤春,李艳玲,田园. 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[J]. 理化检验-化学分册, 2019, 55(4): 442~446
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参考文献
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【2】樊慧婷,林洪生.蛹虫草化学成分及药理作用研究进展[J].中国中药杂志, 2013,38(15):2549-2552.
【3】郑荣,毛丹,王柯,等.HPLC法测定中药中黄曲霉毒素B1、B2、G1、G2的含量[J].药物分析杂志, 2005,25(6):610-613.
【4】刘丽娜,王莹,金红宇,等.HPLC法测定虫草发酵粉中黄曲霉毒素残留量[J].药物分析杂志, 2011,31(7):1256-1259.
【5】黄莉,张浩,丁伟琴,等.中药中真菌毒素污染问题[J].海峡药学, 2009,21(6):95-99.
【6】欧阳佩,徐新军.中药中黄曲霉毒素分析方法进展[J].现代食品与药品杂志, 2007,17(3):12-16.
【7】杨丰利,汤蕾妍,何宝祥.黄曲霉毒素脱毒方法的研究进展[J].广西畜牧兽医, 2006,22(5):223-225.
【8】白璐.黄曲霉毒素的危害[J].吉林农业, 2012(1):178-178.
【9】胡一晨,万丽,范成杰,等.免疫亲和柱净化HPLC柱后光化学衍生化法检测中药及染菌中药制剂中间体的黄曲霉毒素[J].中国实验方剂学杂志, 2012,18(10):116-119.
【10】朱迪,谭丹,向文英,等.免疫亲和柱-HPLC柱后光化学衍生法测定中药饮片中黄曲霉毒素B1、B2、G1、G2的含量[J].贵阳医学院学报, 2015,40(8):843-847.
【11】杨贵芝,刘晓霞,邹建宏,等.富含色素类中药材中黄曲霉毒素的高效液相色谱-荧光检测方法研究[J].食品安全质量检测学报, 2014,5(4):1125-1132.
【12】郝爱鱼,赵丽元,刘英慧,等.HPLC柱后光衍生荧光法测定中药饮片中黄曲霉毒素残留量[J].药物分析杂志, 2012,32(12):2203-2207.
【13】王娅玲,李维峰,刘宝,等.高效液相色谱柱后衍生法测定中药材中的黄曲霉毒素[J].云南化工, 2014,41(1):42-44.
【14】ANASTASSIADES M, LEHOTAY S J, STAJNBAHER D, et al. Fast and easy multiresidue method employing acetonitrile extraction/partitioning and "dispersive solid-phase extraction" for the determination of pesticide residues in produce[J]. Journal of AOAC International, 2003,86(2):412-431.
【15】SIRHAN A Y, TAN G H, WONG R C S. Method validation in the determination of aflatoxins in noodle samples using the QuEChERS method (Quick, Easy, Cheap, Effective, Rugged and Safe) and high performance liquid chromatography coupled to a fluorescence detector (HPLCeFLD)[J]. Food Control, 2011,22(12):1807-1813.
【16】FRENICH A G, ROMERO-GONZÁLEZ R, GÓMEZ-PÉREZ M L, et al. Multi-mycotoxin analysis in eggs using a QuEChERS-based extraction procedure and ultra-high-pressure liquid chromatography coupled to triple quadrupole mass spectrometry[J]. Journal Chromatography A, 2011(1218):4349-4356.
【17】ANNUNZIATA I L, STRAMENGA A, VISCIANO P, et al. Simultaneous determination of aflatoxins, T-2 and HT-2 toxins, and fumonisins in cereal-derived products by QuEChERS extraction coupled with LC-MS/MS[J]. Analytical and Bioanalytical Chemistry, 2017,409(21):5143-5155.
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