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婴幼儿米粉中井冈霉素A残留量的测定

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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20mmol/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(R2>0.99),检出限为2.0 μg/kg,定量限为5.0 μg/kg.在空白婴幼儿米粉样品中进行了5.0、50.0、200.0 μg/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.
Determination of Validamycin A residues in Baby Rice Flour
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(R2>0.99)within the range of 0.1 ng/mL to 5.0 ng/mL.The limits of detection and quantification were 2.0 pg/kg and 5.0 pg/kg,respectively.Recovery experiments spiked at levels of 5.0,50.0,200.0 μg/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.

baby rice flourvalidamycin AMCX solid phase extraction columnhydrophilic interaction chromatography-tandem mass spectrometry

薛霞、胡梅、卢兰香、王骏、魏莉莉、武传香、丁一、刘艳明

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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

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

山东省市场监督管理局科研项目

SDSJKJ202310

2024

食品科技
北京市粮食科学研究所

食品科技

CSTPCD北大核心
影响因子:0.622
ISSN:1005-9989
年,卷(期):2024.49(8)