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高效液相色谱-质谱法测定6种玉米赤霉醇类真菌毒素 被引量:5

Simultaneous Determination of 6 Zearmycotoxins in Foods by High Performance Liquid Chromatography-Tandem Mass Spectrometry
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摘要 利用通过式固相萃取结合高效液相色谱-串联质谱法建立食品中α-玉米赤霉醇、β-玉米赤霉醇、α-玉米赤霉烯醇、β-玉米赤霉烯醇、玉米赤霉酮和玉米赤霉烯酮6种真菌毒素的检测方法。样品酶解后经乙腈提取,通过式固相萃取柱净化,液相色谱-质谱/质谱仪测定,采用同位素内标法定量。6种真菌毒素在曲线浓度范围内(2.5~125 ng/mL)线性关系良好,在2.0, 4.0和20.0μg/kg这3个添加水平的平均回收率为72.6%~110.4%,相对标准偏差为1.8%~14.6%(n=6), 6种真菌毒素的检出限均为1.0μg/kg,定量限均为2.0μg/kg。该方法操作简便、灵敏度高、重复性好、基质干扰小,能有效提高样品的检测效率,适用于食品中6种玉米赤霉醇类真菌毒素的检测。 A method for the determination ofα-zearalenol,β-zearalenol,α-zearalenol,β-zearalenol,zearalenone and zearalenone mycotoxins in foods by pass-through solid phase extraction-high performance liquid chromatography-tandem mass spectrometry(SPE-HPLC-MS/MS)was established.The samples were extracted by acetonitrile after enzymatic hydrolysis,and the extract was purified by pass-through solid phase extraction column and passed through an amide(3.0 mmx100 mm,1.7μm)chromatography column.After separation,it was detected in the multiple reaction monitoring(MRM)mode,and quantitated by an internal standard method.The linear relationships of the six mycotoxins were good in the concentration range of the curve.The average recoveries ranged from 72.6%to 110.4%,and the relative standard deviations were between 1.8%and 14.6%(n-6).The detection limits of 6 mycotoxins were 1.0μg/kg,and the limits of quantification were 2.0μg/kg.The method is simple,sensitive and repeatable,and has low matrix interference,which can effectively improve the detection eficiency of samples,and is suitable for the detection of 6 zearzol mycotoxins in food.
作者 吴雪莹 戴琴 付睿婕 黄婷 肖全伟 宋娟 WU Xueying;DAI Qin;FU Ruijie;HUANG Ting;XIAO Quanwei;SONG Juan(Chengdu Institute of Food Inspection,Chengdu 611130;Key Laboratory of Chemical Metrology and Applications on Nutrition and Health for State Market Regulation,Beijing 100029)
出处 《食品工业》 CAS 2024年第7期296-301,共6页 The Food Industry
基金 国家重点研发计划(2022YFF0710405)资助 国家市场监督管理总局项目(2021YJ009)资助 四川省科技计划项目(2022YFS0511)资助 国家市场监管重点实验室(调味品监管技术)开放课题(KLCST-2022-03)资助。
关键词 固相萃取 真菌毒素 高效液相色谱-串联质谱 食品 solid phase extraction mycotoxin high performance liquid chromatography-tandem mass spectrometry food
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