高效液相色谱串联质谱法测定红糖中3-硝基丙酸  

Determination of 3-Nitropropionic Acid in Brown Sugar by HPLC-MS/MS

作　　者：高裕锋 庞扬海 甄振鹏 黄敏兴 余构彬 郭剑雄 GAO Yu-feng;PANG Yang-hai;ZHEN Zhen-peng;HUANG Min-xing;YU Gou-bin;GUO Jian-xiong(Guangdong Provincial Bioengineering Institute (Guangzhou Sugarcane Industry Research Institute)/Guangdong Key Lab of Sugarcane Improvement & Biorefinery,Guangzhou 510316;China Sugar Inspection Center,Guangzhou 510316)

机构地区：[1]广东省生物工程研究所(广州甘蔗糖业研究所)广东省甘蔗改良与生物炼制重点实验室,广东广州510316 [2]国家糖业质量监督检验中心,广东广州510316

出　　处：《甘蔗糖业》2019年第3期56-59,共4页Sugarcane and Canesugar

基　　金：广州市科技计划项目(201806010093);广东省科技计划项目(2016A040403066)

摘　　要：建立了红糖中3-硝基丙酸的高效液相色谱串联质谱检测方法。红糖样品用乙醇-水溶解,涡旋振荡,离心后取上清液,用PWAX固相萃取柱净化,氮气吹干洗脱液,甲醇-甲酸水复溶后,用高效液相色谱串联质谱检测。采用Luma Omega C18柱(1.6μm,100mm×2.1mm),以甲醇和水为流动相进行分离,电喷雾负离子模式(ESI-),多反应监测(MRM)检测,外标法定量。结果表明,3-硝基丙酸在0.1~20μg/L浓度范围内线性关系良好(r=1.0000),该方法的检出限为0.057μg/kg,定量限为0.189μg/kg。在2.5、10、50μg/kg的加标水平下,3-硝基丙酸的平均回收率为79.2%~85.5%,相对标准偏差为5.2%~7.3%以下(n=6)。本方法操作简单、灵敏度高、结果准确,可用于红糖中3-硝基丙酸的残留量测定。A method was developed for the determination of 3-nitropropionic acid in brown sugar by High Performance Liquid Chromatography Tandem Mass Spectrometry(HPLC-MS/MS).The sugar samples were extracted by ethanol-water solution,then vortex and centrifugate.The extracted solution was purified by the PWAX solid-phase extraction column,then the purified solution was concentrated by nitrogen,used methanol-water(0.1%formic acid)to dissolve.Chromatographic separation was achieved on Luma Omega C18 column(1.6μm,100 mm×2.1 mm).The mobile phase consisted of water and methanol,then analyzed by using HPLC-MS/MS in multiple reaction monitoring(MRM)mode via negative electrospray ionization.External standard method was used to determine 3-nitropropionic acid contents(0.1~20μg/L)with a good linear relationship(r=1.0000).The limit of quantification(LOQ)was 0.057μg/kg,the limit of quantification was 0.189μg/kg.The recoveries of acrylamide at three levels of 2.5,10,and 50μg/kg were from 79.2%to 85.5%with the relative standard deviations(RSDs)of 5.2%~7.3%(n=6)in brown sugar.The method was simple and characterized with acceptable sensitivity and accuracy to meet the requirements of the determination of 3-nitropropionic acid in brown sugar.

关 键 词：红糖 3-硝基丙酸 高效液相色谱串联质谱法 

分 类 号：TS247[轻工技术与工程—制糖工程]