高效液相色谱串联质谱法测定乳粉中低聚果糖  

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

作　　者：甄振鹏[1,2] 高裕锋[1,2] 庞扬海 黄敏兴[1,2] 王小鹏[1,2] 余构彬[1,2] 郭剑雄[1,2] 

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》2017年第4期59-63,共5页Sugarcane and Canesugar

基　　金：广东省科技计划项目(2013B040400003;2013B061800023;2013B061800007;2014B040404054;2016A040403066);广东省科学院项目(2016GDASPT-010)

摘　　要：建立了测定乳粉中低聚果糖(蔗果三糖、蔗果四糖、蔗果五糖、蔗果六糖)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XBridge TM Amide(3.5μm,4.6 mm×150 mm)柱,以乙腈-氨水溶液为流动相进行洗脱,电喷雾质谱负离子(ESI-),多反应监测(MRM)模式检测,外标法定量。该方法在0.5~20 mg/L范围线性良好(r>0.9990,检出限最低为0.022 mg/kg)。分别在样品中添加标准物质1、5、10 mg/kg进行回收率实验,方法的回收率范围为90.8%~95.8%,相对标准偏差为3.6%~9.0%(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果糖的检测要求。A method was developed for the determination of fructo-oligosaccharides （FOS） 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 XBridge TM Amide column （3.5 ~tm, 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 0.5-20 mg/L （r〉0.9990）. The limit of quantification （LOQ） was 0.022 mg/kg. The standard substance of 1, 5, 10 mg/kg was added to the samples in the recovery test, the results showed that the recovery rate was in the range of 90.8%-95.8% and the relative standard deviation was 3.6%-9.0% （n=6）. The method was simple, rapid and characterized with acceptable sensitivity and accuracy to meet the requirement of the detection of FOS in milk powder.

关 键 词：乳粉 低聚果糖 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]