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新型在线净化前处理HPLC-MS/MS测定香精香料中的麦角甾醇和麦角甾酮 预览 被引量:1

Novel Online Purification Pretreatment System Coupled with HPLC-MS/MS for Determination of Ergosterol and Ergotsterone in Food Flavors and Spices
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摘要 建立一种新型的在线净化前处理装置结合高效液相色谱-串联质谱(high performance liquid chromatography-tandem with mass spectrometry,HPLC-MS/MS)法测定香精香料中的麦角甾醇和麦角甾酮。该前处理装置结合基质分散萃取和柱层析对样品进行萃取和净化,之后对样品进行浓缩并利用HPLC-MS/MS分析测定。HPLC-MS/MS方法以甲醇和水为流动相,0.4 mL/min流速条件下梯度洗脱,采用C18色谱柱进行液相色谱分离,大气压正离子方式电离,多重反应监测模式检测,内标法进行定量分析。结果表明,该方法前处理方便且稳定性强,溶剂可回收,净化萃取浓缩为一体;目标物质麦角甾醇和麦角甾酮能在5 min内得到分离检测,在1.5~250μg/m L范围内具有较好的线性,各待测物的线性相关系数均大于0.999,检出限为0.32~0.35μg/mL,在不同添加水平条件下,平均回收率为86%~96%,相对标准偏差在3.1%~3.6%之间。本方法能较好地应用于香精香料实际样品中麦角甾醇和麦角甾酮的测定。 A method using a new online purifying pretreatment system and high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)was established for the determination of ergosterol and ergotsterone in food flavors and spices.The pretreatment method in combination with matrix solid-phase dispersion and column chromatography was used for sample extraction and purification,followed by concentration and analysis by HPLC-MS/MS.The analysis was performed on a C18 column with gradient elution with a mobile phase consisting of water and methanol at a flow rate of0.4 mL/min.The mass spectrometer with an atmospheric pressure chemical ionization(APCI)source in the positive ion mode was operated using multiple reaction monitoring(MRM)and an internal standard method was used for quantification.The results showed that the pretreatment method was simple and stable with solvent recycle,integrating extraction,purification and concentration.The two analytes could be separated in 5 min with good linearity in the concentration range of1.5–250μg/m L with correlation coefficients larger than 0.999.The limits of detection(LODs)were 0.32μg/mL for ergosterol and 0.35μg/mL for ergotsterone.The mean recoveries of the target compounds at three different spiked levels were 86%–96%with relative deviations(RSDs)of 3.1%–3.6%.This method is suitable for the analysis of ergosterol and ergotsterone in food flavors and spices.
作者 李晶 倪朝敏 陈建华 米其利 孔维松 王晓辉 杨光宇 李雪梅 杨叶昆 LI Jing, NI Chaomin, CHEN Jianhua, MI Qili, KONG Weisong, WANG Xiaohui, YANG Guangyu, LI Xuemei, YANG Yekun(Center of Technology, China Tobacco Yunnan Industrial Co. Ltd., Kunming 650106, China)
出处 《食品科学》 CSCD 北大核心 2018年第12期313-318,共6页 Food Science
基金 中国烟草总公司科研重点项目(110201502006) 云南中烟工业有限责任公司科技项目(2018JC07)
关键词 麦角甾醇 麦角甾酮 在线净化前处理 高效液相色谱-串联质谱 香精香料 ergosterol ergotsteron online purification pretreatment HPLC-MS/MS flavors and spices
作者简介 李晶(1982-),女,助理研究员,博士,研究方向为色谱质谱分析.E-mail:lijing_1107@163.com;通信作者:杨叶昆(1972-),男,副研究员,博士,研究方向为烟用香精香料制备.E-mail:yangyekun@163.com
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