婴幼儿米粉中井冈霉素A残留量的测定  

Determination of Validamycin A residues in Baby Rice Flour

作　　者：薛霞 胡梅 卢兰香 王骏 魏莉莉 武传香 丁一 刘艳明 XUE Xia;HU Mei;LU Lanxiang;WANG Jun;WEI Lili;WU Chuanxiang;DING Yi;LIU Yanming(Shandong Institute for Food and Drug Control,Key Laboratory of Supervising Technology for Meat and Meat Products,State Administration for Market Regulation,Industrial Technology Foundation Public Service Plateform,Jinan 250101,China)

机构地区：[1]山东省食品药品检验研究院国家市场监督管理总局重点实验室(肉及肉制品重点监管技术)产业技术基础公共服务平台,山东济南250101

出　　处：《食品科技》2024年第8期316-321,共6页Food Science and Technology

基　　金：山东省市场监督管理局科研项目(SDSJKJ202310)。

摘　　要：文章建立了亲水作用色谱-串联质谱法测定婴幼儿米粉中井冈霉素A残留量的分析方法。采用甲醇-水(7:3)作为溶剂进行目标物的提取,取1 mL提取液氮吹干后用20 mmol/L醋酸铵(pH3.0)复溶,MCX固相萃取柱净化,以5 mmol/L醋酸铵和乙腈为流动相,经BEH Amide色谱柱分离后采用电喷雾质谱多反应监测方式扫描,外标法定量。结果表明,该方法在0.1~5.0 ng/mL范围内线性关系良好(R^(2)>0.99),检出限为2.0μg/kg,定量限为5.0μg/kg。在空白婴幼儿米粉样品中进行了5.0、50.0、200.0μg/kg 3个浓度水平的加标回收实验,方法的平均回收率为88.5%~100.5%,相对标准偏差为4.84%~10.08%。所建方法的提取及净化过程简便、重现性好、灵敏度高,可用于的婴幼儿米粉中井冈霉素A的快速定性定量分析。An analytical method was developed for the determination of validamycin A in baby rice flour by hydrophilic interaction liquid chromatography coupled with tandem-mass spectrometry.The target compound was extracted with methanol-water(7:3),1 mL of the extract solution was evaporated to dry under nitrogen flow,then redissolved in 20 mmol/L ammonium acetate(pH3.0)and cleaned-up with MCX solid phase extraction column.The separation was carried out on a BEH Amide column using 5 mmol/L ammonium acetate-acetonitrile as mobile phase and detection was performed using electrospray ionization mass spectrometry in multiple reaction monitoring mode,with quantification done using the external standard method.The method showed good linearity(R^(2)>0.99)within the range of 0.1 ng/mL to 5.0 ng/mL.The limits of detection and quantification were 2.0μg/kg and 5.0μg/kg,respectively.Recovery experiments spiked at levels of 5.0,50.0,200.0μg/kg in blank baby rice flour yielded average recoveries of 88.5%to 100.5%,with relative standard deviations of 4.84%to 10.08%.The method is characterized by its simplicity in extraction and purification,good reproducibility,and high sensitivity,making it suitable for the rapid qualitative and quantitative analysis of validamycin A in baby rice flour.

关 键 词：婴幼儿米粉 井冈霉素A MCX固相萃取柱 亲水作用色谱-串联质谱法 

分 类 号：TS207.53[轻工技术与工程—食品科学]