摘要
该文以酵素梅为实验基质,采用超高效液相色谱-串联质谱(UPLC-MS/MS)建立了一种能够快速、准确测定酵素梅中酚丁及其9种酯类衍生物(双醋酚丁、双丙酚丁、双环丙酚丁、双丁酚丁、双戊酚丁、双己酚丁、双环己甲酰酚丁、双庚酚丁、双辛酚丁)和5种类似物(双酚沙丁、4-氯酚丁、双酚沙丁醋酸酯、4-氯双醋酚丁、三醋酚丁)含量的方法。样品经甲醇超声提取,离心、定容后,利用Waters Acquity BEH C18柱(50mm×2.1 mm,1.7μm)进行分离,以5 mmol/L醋酸铵水溶液-乙腈为流动相进行梯度洗脱,采用电喷雾电离源正离子多反应监测模式进行扫描,基质匹配外标法定量分析。15种化合物在一定质量浓度范围内线性关系良好,相关系数(r^(2))为0.998 1~0.999 9,方法检出限为0.005~0.025 mg/kg,定量下限为0.015~0.075 mg/kg,各化合物的加标回收率为72.8%~114%,相对标准偏差为1.1%~9.0%。采用该方法对10份不同来源的酵素梅进行检测,共检出9种化合物,分别为酚丁、双丙酚丁、双丁酚丁、双戊酚丁、双己酚丁、双环己甲酰酚丁、双醋沙丁、4-氯酚丁、4-氯双醋酚丁,含量在0.1~851.9 mg/kg之间。该法准确、灵敏、快速,适用于酵素梅中酚丁及其酯类衍生物和类似物含量的检测。
In this study,a novel method for the simultaneous detection and quantification of oxyphenisatin,its nine ester derivatives(oxyphenisatine diacetate,oxyphenisatine dipropionate,dicyclopropafenedine,oxyphenisatine dibutyrate,oxyphenisatine divalerate,oxyphenisatine dihexylester,dicyclohexylphenol butyl,oxyphenisatine dienanthate and oxyphenisatine dioctanoate),and five analogues(bisoxatin,4-chloro-oxyphenisatine,bisoxatin acetate,4-chloro-oxyphenisatine diacetate and triacetyldiphenolisatin)in ferment plum using ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).The sample was ultrasonically extracted with methanol,volume fixed and centrifuged.The separation was performed by Waters Acquity BEH C18 column(50 mm×2.1 mm,1.7μm)by gradient elution with 5 mmol/L ammonium acetate aqueous solution and acetonitrile as mobile phases.The compounds were step scanned using an electrospray ionization source in the positive and multiple reaction monitoring(MRM)modes,and analyzed by matrix matched external standard method.The results showed that 15 compounds achieved great linearity in the linear ranges,with a correlation coefficients(r^(2))not less than 0.9981.The limits of detection(LODs)of 15 compounds ranged from 0.005 to 0.025 mg/kg,and the limits of quantification(LOQs)ranged from 0.015 to 0.075 mg/kg.The average recoveries ranged from 72.8%to 114%,while the relative standard deviations(RSDs)were between 1.1%to 9.0%.The method was successfully applied to the determination of 10 fermenter plum samples obtained from different Taobao shops.A total of 9 illegal adulterants were detected,namely oxyphenisatin,oxyphenisatinedipropionate,oxyphenisatine dibutyrate,oxyphenisatinedivalerate,oxyphenisatine dihexylester,dicyclohexylphenol butyl,bisoxatin,4-chloro-oxyphenisatine,4-chloro-oxyphenisatine diacetate.The contents ranged from 0.1 to 851.9 mg/kg.The method is accurate,sensitive,rapid,and it is suitable for detection of the 15 illegal adulterants in ferment plum.
作者
夏宝林
扈战强
张亚清
殷晶晶
汪仕韬
杨娜
张维益
XIA Bao-lin;HU Zhan-qiang;ZHANG Ya-qing;YIN Jing-jing;WANG Shi-tao;YANG Na;ZHANG Wei-yi(Jiangyin Food Safety Testing Center,Jiangyin 214400,China;School of Food and Pharmacy,Shanghai Zhongqiao Vocational and Technical University,Shanghai 201514,China)
出处
《分析测试学报》
北大核心
2025年第3期493-499,共7页
Journal of Instrumental Analysis
基金
江阴市社会发展科技示范项目(JY0603A011014230014PB,JY0603A011014230027PB)
上海中侨职业技术大学校级课题(ZQZR202439)。
关键词
酚丁
酯类衍生物
类似物
超高效液相色谱-串联质谱
酵素梅
oxyphenisatin
ester derivatives
analogues
ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)
ferment plum
作者简介
通讯作者:扈战强,博士,助理研究员,研究方向:食品安全检测技术,E-mail:hzq8362029@163.com。
