在线固相萃取-毛细管高效液相色谱联用测定奶酪中的生物胺

引用本文: 杨姗姗, 杨亚楠, 李雪霖, 张燕. 在线固相萃取-毛细管高效液相色谱联用测定奶酪中的生物胺[J]. 分析化学, 2016, 44(3): 396-402. doi: 10.11895/j.issn.0253-3820.150811 shu

Citation: YANG Shan-Shan, YANG Ya-Nan, LI Xue-Lin, ZHANG Yan. Determination of Biogenic Amines in Cheese by On-line Solid Phase Extraction Coupled with Capillary High Performance Liquid Chromatography[J]. Chinese Journal of Analytical Chemistry, 2016, 44(3): 396-402. doi: 10.11895/j.issn.0253-3820.150811 shu

在线固相萃取-毛细管高效液相色谱联用测定奶酪中的生物胺

1.
食品营养与安全教育部重点实验室, 天津科技大学, 天津 300457

通讯作者: 张燕

基金项目:
本文系国家高技术研究发展计划基金资助项目(863计划,No.2011AA100807) (863计划,No.2011AA100807)

摘要: 采用双二元泵毛细管液相色谱,通过六通阀实现了样品的在线净化与分离定量的自动切换,建立了同时测定奶酪中的15种生物胺的在线固相萃取-毛细管高效液相色谱联用方法。通过优化毛细管高效液相色谱的分离条件,考察在线固相萃取流动相的组成、上样溶液pH值以及六通阀的切换时间对生物胺回收率的影响,确定最佳分析条件为:5%乙腈-水作为固萃柱(Zorbax SB-C₁₈)的流动相,上样溶液pH=11,上样3 min后切换六通阀。采用内标法定量,15种生物胺标准曲线的线性范围为0.25~50.0 mg/L,检出限(LOD)为0.05~0.25 mg/L,定量限(LOQ)为0.15~0.80 mg/L。除了甲胺、乙胺、3-甲基丁胺和5-羟基色胺外,其余生物胺的不同添加水平(1, 20和40 mg/kg)下的加标回收率为79.6%~118.7%; 除3-甲基丁胺和5-羟基色胺外,其余生物胺的RSD在0.3%~14.9%之间,可用于奶酪中多种生物胺的快速检测。

关键词:

English

Determination of Biogenic Amines in Cheese by On-line Solid Phase Extraction Coupled with Capillary High Performance Liquid Chromatography

1.
Key Laboratory of Food Nutrition and Safety, Ministry of Education of China, Tianjin University of Science and Technology, Tianjin 300457, China

Corresponding author: 张燕

Received Date: 15 October 2015
Fund Project:
本文系国家高技术研究发展计划基金资助项目(863计划,No.2011AA100807)

Abstract: An on-line solid phase extraction coupled with capillary HPLC method was established for the simultaneous determination of fifteen kinds of biologic amines in cheese. The biogenic amines were concentrated on the solid phase extraction column, and transferred by the six-way valve to analytical column for separation and detection. Separation conditions on capillary HPLC, composition of on-line SPE mobile phase, pH of the sample solution and switching time of six-way switching valve were investigated to get better separation conditions of 15 biogenic amines. Optimum on-line SPE conditions including 5% of the acetonitrile-water as mobile phase for SPE column, pH=11 of the sample solution and 3 min of valve switching time were employed in the analytical method. The linear range of standard curve for fifteen biogenic amines was 0.25-50.0 mg/L; LOD were within the range of 0.05-0.25 mg/L. At spiked levels of 1, 20, 40 mg/kg, the recoveries of fifteen biogenic amines on four kinds of cheese ranged from 79.6% to 118.7% except methylamine, ethylamine, 3-methylbutanamine and 5-hydroxytryptamine; with RSDs from 0.3% to 14.9% except 3-methylbutanamine and 5-hydroxy-tryptamine. The method is accurate and reliable, and can be used to detect biogenic amines in cheese.

Key words:

On-line solid phase extraction
/ Capillary high performance liquid chromatography
/ Biogenic amines
/ Cheese

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1.
沈阳化工大学材料科学与工程学院沈阳 110142

在线固相萃取-毛细管高效液相色谱联用测定奶酪中的生物胺

通讯作者: 张燕

English

Determination of Biogenic Amines in Cheese by On-line Solid Phase Extraction Coupled with Capillary High Performance Liquid Chromatography

Corresponding author: 张燕

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通讯作者: 陈斌, bchen63@163.com

中国化学会秘书处

在线固相萃取-毛细管高效液相色谱联用测定奶酪中的生物胺

通讯作者: 张燕

English

Determination of Biogenic Amines in Cheese by On-line Solid Phase Extraction Coupled with Capillary High Performance Liquid Chromatography

Corresponding author: 张燕

CCS Chemistry：嵌段共聚物自组装成 “三明治”二维有机材料，实现纳米级压力传感功能

CCS Chemistry：颜徐州、鲍哲南： 你的皮肤可能是一片SPMs

CCS Chemistry：工作高效不疲劳，只须让催化剂动起来

CCS Chemistry：静电组装导向聚合- 聚电解质纳米凝胶量化制备新策略

CCS Chemistry：金黄色葡萄球菌醛基脱氢酶是如何识别特异性底物的？

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通讯作者: 陈斌, bchen63@163.com

中国化学会秘书处

CCS Chemistry：颜徐州、鲍哲南：你的皮肤可能是一片SPMs