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

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.