多壁碳纳米管净化-超高效液相色谱-质谱法测定水产品中头孢菌素残留量

引用本文: 顾蓓乔, 梅光明, 张小军, 何依娜, 严忠雍, 朱敬萍. 多壁碳纳米管净化-超高效液相色谱-质谱法测定水产品中头孢菌素残留量[J]. 分析化学, 2017, 45(3): 381-388. doi: 10.11895/j.issn.0253-3820.160633 shu

Citation: GU Bei-Qiao, MEI Guang-Ming, ZHANG Xiao-Jun, HE Yi-Na, YAN Zhong-Yong, ZHU Jing-Ping. Determination of 8 Kinds of Cephalosporins in Aquatic Products by Multi-walled Carbon Nanotubes Solid Phase Extraction-Ultra High Performance Liquid Chromatography-Mass Spectrometry[J]. Chinese Journal of Analytical Chemistry, 2017, 45(3): 381-388. doi: 10.11895/j.issn.0253-3820.160633 shu

多壁碳纳米管净化-超高效液相色谱-质谱法测定水产品中头孢菌素残留量

浙江省海洋水产研究所, 浙江省海水增养殖重点实验室, 舟山 316021
基金项目:
本文系浙江省科技厅计划项目(Nos.2016C32074，2016F30022)资助

摘要: 建立了水产品可食部位中头孢哌酮、头孢喹肟、头孢洛宁、头孢唑啉、头孢匹林、头孢噻呋、头孢匹罗和头孢氨苄8种头孢菌素的超高效液相色谱-质谱测定法。样品经乙腈-水溶液提取、多壁碳纳米管固相萃取净化后，以Acquity Xselect CSH C₁₈柱为分离柱，用乙腈和0.1%甲酸溶液进行梯度洗脱，电喷雾正离子多反应模式监测。结果表明，8种头孢菌素均呈良好的线性关系(R²≥0.995)，定量限(S/N=10)在2-10 μg/kg之间；在阴性样品采取梯度加标，添加回收率为67.3%~94.2%，RSD为3.3%~14%。本方法检测成本低、准确度高、精密度好，能够满足水产品中头孢菌素检测的要求。

关键词:

English

Determination of 8 Kinds of Cephalosporins in Aquatic Products by Multi-walled Carbon Nanotubes Solid Phase Extraction-Ultra High Performance Liquid Chromatography-Mass Spectrometry

Marine Fisheries Research Institute of Zhejiang, Key Lab of Mariculture and Enhancement of Zhejiang Province, Zhoushan 316021, China
Received Date: 23 August 2016
Revised Date: 23 November 2016
Fund Project:
This work was supported by the Science & Technology Department Project of Zhejiang Province, China (Nos. 2016C32074, 2016F30022)

Abstract: An ultra-high performance liquid chromatography-mass spectrometry (UPLC-MS/MS) method was developed for the determination of 8 kinds of cephalosporins, cefoperazone, cefquinome, cefalonium, cefazolin, cefapirin, Ceftiofur, cefpirome and cefalexin, in edible parts of aquatic products. The samples were extracted with acetonitrile-water and cleaned up by multi-walled carbon nanotubes (MWCNTs) SPE cartridge. All the target compounds were separated on an Acquity Xselect CSH C₁₈ column with gradient elution by using acetonitrile and 0.1% formic acid aqueous as eluent, and detected by UPLC-MS/MS under ESI⁺ ionization and MRM mode. Under optimized conditions, this method had a good linearity (R²≥0.995) and the limits of quantification were in the range of 2-10 μg/kg (S/N=10). The recoveries of the method for the target compounds spiked at three different levels were 67.3%-94.2% with the relative standard deviations (RSDs) of 3.3%-14%. The method had the characteristics of low cost, high accuracy and good precision, and could meet the requirements of cephalosporins determination.

Key words:

Multi-walled carbon nanotubes
/ Ultra-high performance liquid chromatography-mass spectrometry
/ Aquatic product
/ Cephalosporins

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1.
沈阳化工大学材料科学与工程学院沈阳 110142

多壁碳纳米管净化-超高效液相色谱-质谱法测定水产品中头孢菌素残留量

English

Determination of 8 Kinds of Cephalosporins in Aquatic Products by Multi-walled Carbon Nanotubes Solid Phase Extraction-Ultra High Performance Liquid Chromatography-Mass Spectrometry

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通讯作者: 陈斌, bchen63@163.com

中国化学会秘书处

多壁碳纳米管净化-超高效液相色谱-质谱法测定水产品中头孢菌素残留量

English

Determination of 8 Kinds of Cephalosporins in Aquatic Products by Multi-walled Carbon Nanotubes Solid Phase Extraction-Ultra High Performance Liquid Chromatography-Mass Spectrometry

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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