高效液相色谱串联质谱法测定乳粉中低聚半乳糖  

Determination of GOS in Milk Powder by HPLC-MS/MS

作　　者：甄振鹏 高裕锋 黄敏兴 庞扬海 王小鹏 李硕聪 余构彬 ZHEN Zhen-peng;GAO Yu-feng;HUANG Min-xing;PANG Yang-hai;WANG Xiao-peng;LI Shuo-cong;YU Gou-bin(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1期46-50,共5页Sugarcane and Canesugar

基　　金：广东省科技计划项目(2016A040403066);广州市科技计划项目(201806010093);广东省科学院项目(2016GDASPT-010)

摘　　要：建立了乳粉中棉籽糖、水苏糖、毛蕊花糖等低聚半乳糖的高效液相色谱串联质谱(HPLC-MS/MS)检测方法。乳粉样品用乙醇水提取,上清液稀释后,采用XBridgeTM Amide (3.5μm,4.6 mm×150 mm)柱,以乙腈水溶液为流动相进行洗脱,电喷雾质谱负离子模式(ESI-),多反应监测(MRM)检测,外标法定量。该方法在50～1500μg/L线性良好(r>0.9986,检出限最低为7.7μg/kg)。分别在空白样品中添加标准物质100、500、1000μg/kg进行回收率实验,方法的回收率范围为80.8%～86.6%,相对标准偏差为3.0%～8.0%(n=6)。该方法样品前处理简单、快速,分析时间短,灵敏度、准确度和精密度均满足乳粉中低聚半乳糖的检测要求。A method was developed for the determination of galactooligosaccharides(GOS)such as raffinose,stachyose and verbascose in milk powder by High Performance Liquid Chromatography Tandem Mass Spectrometry(HPLC-MS/MS).The samples were extracted by ethanol-water mixed solution,and then centrifugated.Chromatographic separation was achieved on XBridgeTM Amide column(3.5μm,4.6 mm×150 mm).The mobile phase consisted of acetonitrile-ammonia solution,and then analyzed by using HPLC-MS/MS in multiple reaction monitoring(MRM)mode on negative electrospray ionization(ESI-).External standard method was used to determine the residue contents with a good linear relationship of 50~1500μg/L(r >0.9986).The limit of quantification(LOQ)was 7.7μg/kg.The standard substance of 100,500,1000μg/kg was added to the samples in the recovery test,the results showed that the recovery rate was in the range of 80.8%~86.6%and the relative standard deviation was 3.0%~8.0%(n=6).The method was simple,rapid and characterized with acceptable sensitivity and accuracy to meet the requirement of the detection of GOS in milk powder.

关 键 词：乳粉 低聚半乳糖 高效液相色谱串联质谱法 

分 类 号：TS245.4[轻工技术与工程—制糖工程]