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作 者:李灿 陈同强 汪辉 李政 谢芳云 向俊 王云昊 王亮亮 LI Can;CHEN Tong-qiang;WANG Hui;LI Zheng;XIE Fang-yun;XIANG Jun;WANG Yun-hao;WANG Liang-liang(Hunan Provincial Key Laboratory of Food Safety Monitoring and Early Warning,Hunan Provincial Institute of Product and Goods Quality Inspection,Changsha 410017,China;Changsha Institute for Food and Drug Control,Changsha 410016,China)
机构地区:[1]湖南省产商品质量检验研究院,食品安全监测与预警湖南省重点实验室,湖南长沙410017 [2]长沙市食品药品检验所,湖南长沙410016
出 处:《分析测试学报》2025年第3期500-505,共6页Journal of Instrumental Analysis
基 金:湖南省市场监督管理局科技项目(2024KJJH34);湖南省自然科学基金(2022JJ90026,2023JJ60533)。
摘 要:建立了高效液相色谱-串联质谱快速筛查和确证酵素源食品中9种酚汀和酚酞及其衍生物的方法。样品采用乙腈-水涡旋振荡提取,离心后取上清液过滤膜。采用Hypersil Gold C_(18)柱进行分离,0.1%甲酸水溶液和0.1%甲酸乙腈为流动相梯度洗脱,在电喷雾离子源的正离子电离模式下扫描,多反应监测(MRM)模式采集测定,基质匹配外标法定量分析。结果表明:9种目标物在5~100μg/L范围内呈现良好的线性关系,相关系数均不小于0.999 0,方法定量下限为0.05 mg/kg,平均回收率为80.4%~101%,相对标准偏差为1.2%~7.8%。该方法简便快速、前处理简单、灵敏、准确,适用于酵素源食品中9种酚汀和酚酞及其衍生物的批量检测。A new high performance liquid chromatography-tandem mass spectrometry method for screening and confirmation of the oxyphenisatin,phenolphthalein and their derivants in enzyme food was developed.The sample was extracted with acetonitrile-water,followed by centrifugation.The supernatant was then filtered through a membrane filter.The separation was performed on Hypersil Gold C_(18) column with gradient elution with 0.1%formic acid aqueous solution and 0.1%formic acid acetonitrile as mobile phases.The target compounds were determined by positive electrospray ionization under the multiple reaction monitoring(MRM)mode,which quantitative analysis by external standard method with matrix curve.Nine analytes showed good linear relationships in the range of 5-100μg/L with correlation coefficients not less than 0.9990.The results showed that the limit of quantification was 0.05 mg/kg.The average spiked recoveries showed a variation from 80.4%-101%for the three fortification levels,with relative standard deviations between 1.2% and 7.8%.This procedure was noticeably simple,rapid,sensitive and accurate.Therefore,this method is suitable for batch determination of the nine oxyphenisatin,phenolphthalein and their derivants in enzyme food.
关 键 词:酚汀 酚酞 衍生物 高效液相色谱-串联质谱法 酵素源食品
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