色谱

色谱

• 研究论文 • 上一篇    下一篇

高效液相色谱-二极管阵列检测法及高效液相色谱-电喷雾串联质谱法测定植物源性蛋白中残留的三聚氰胺

丁涛1,徐锦忠1,李健忠2,沈崇钰1,吴斌1,陈惠兰1,李淑娟2

  

  1. 1.Animal, Plant and Food Inspection Center of Jiangsu Entry-Exit Inspection and Quarantine Bureau, Nanjing 210001, China;
    2.Chinese Academy of Inspection and Quarantine, Beijing 100025, China
  • 收稿日期:2007-06-22 修回日期:2007-08-21 出版日期:2008-01-30 发布日期:1984-09-25
  • 通讯作者: 丁涛

Determination of melamine residue in plant origin protein powders using high performance liquid chromatography-diode array detection and high performance liquid chromatography-electrospray ionization
tandem mass spectrometry

DING Tao1, XU Jinzhong1, LI Jianzhong2, SHEN Chongyu1,
WU Bin1, CHEN Huilan1, LI Shujuan2   

  1. 1.Animal, Plant and Food Inspection Center of Jiangsu Entry-Exit Inspection and Quarantine Bureau, Nanjing 210001, China;
    2.Chinese Academy of Inspection and Quarantine, Beijing 100025, China
  • Received:2007-06-22 Revised:2007-08-21 Online:2008-01-30 Published:1984-09-25

PDF

2711

摘要：

建立了高效液相色谱-二极管阵列检测器(HPLC-DAD)及HPLC-电喷雾串联质谱(ESI-MS/MS)测定植物源性蛋白中残留的三聚氰胺的方法。利用HPLC-DAD进行样品中三聚氰胺的初筛，利用HPLC-MS/MS进行确证。采用三氯乙酸溶液沉淀样品中的蛋白,同时提取目标分析物,质谱检测时样品再经强阳离子固相萃取柱富集净化。HPLC-DAD的检测低限为10 mg/kg,HPLC-MS/MS的检测低限为0.5 mg/kg;HPLC-DA的添加回收率为76%～88%,HPLC-MS/MS的添加回收率为72%～82%(基质匹配曲线校正)，两种方法的添加回收率的相对标准偏差(RSD)为3.4%～6.4%。

关键词: 高效液相色谱-电喷雾串联质谱, 高效液相色谱-二极管阵列检测, 三聚氰胺残留, 植物源性蛋白

Abstract:

A method for the determination of melamine residue in plant origin protein powders was developed using high performance liquid chromatography-diode array detection (HPLC-DAD) and HPLC-electrospray ionization tandem mass spectrometry (ESI-MS/MS). HPL-DAD was used in preliminary screening of the samples for melamine, and HPLC-MS/MS was used in the confirmatory of melamine. Trichloroacetic acid solution was used to precipitate proteins and to dissociate the target analyte from the sample matrix. The supernatant was cleaned up with strong cation exchange column for HPLC-MS/MS. The HPLC-DAD separation was carried out on a C18 column (250 mm×4.6 mm, 5 μm) with 0.01 mol/L sodium n-heptanesulfate （pH adjusted to 4.5 with citric acid）-acetonitrile (90:10, v/v) as mobile phase at a flow rate of 1.0 mL/min, and detected at 240 nm. HPLC-MS/MS was performed in selected ion monitoring mode with trichloroacetic acid solution as ion pair reagent. The limits of detection were 10 mg/kg and 0.5 mg/kg for HPLC-DAD and HPLC-MS/MS, respectively. The mean recoveries were 76%-88% for HPLC-DAD and 72%-82%(matrix match calibration curve) for HPLC-MS/MS and the relative standard deviations were 3.4%-6.4% for both HPLC-DAD and HPLC-MS/MS.

Key words: high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS), melamine residue, plant origin protein , high performance liquid chromatography-diode array detection (HPLC-DAD)