色谱

色谱 ›› 2020, Vol. 38 ›› Issue (6): 655-662.DOI: 10.3724/SP.J.1123.2019.10011

• 研究论文 • 上一篇    下一篇

QuEChERS-超高效液相色谱-四极杆/静电场轨道离子阱质谱法检测鱼肉中15种降血脂药

王佳1,2, 凌云2, 邓亚美2, 张雨佳2, 杨旭升2, 刘利侠2, 刘晓敏2, 李东辉1,*(), 张峰2,*()   

  1. 1 锦州医科大学药学院, 辽宁 锦州 121001
    2 中国检验检疫科学研究院食品安全研究所, 北京 100176
  • 收稿日期:2019-10-14 出版日期:2020-06-08 发布日期:2020-12-10
  • 通讯作者: 李东辉,张峰
  • 作者简介:张峰.E-mail:fengzhang@126.com
    李东辉.E-mail:lidonghuilx@sina.com;
  • 基金资助:
    国家重点研发计划(2017YFC1601600);国家"万人计划"科技创新领军人才项目（张峰）

Determination of 15 lipid regulators in fish meat by QuEChERS-ultra performance liquid chromatography-quadrupole/ electrostatic field orbitrap mass spectrometry

WANG Jia1,2, LING Yun2, DENG Yamei2, ZHANG Yujia2, YANG Xusheng2, LIU Lixia2, LIU Xiaomin2, LI Donghui1,*(), ZHANG Feng2,*()   

  1. 1 School of Pharmacy, Jinzhou Medical University, Jinzhou 121001, China
    2 Institute of Food Safety, Chinese Academy of Inspection & Quarantine, Beijing 100176, China
  • Received:2019-10-14 Online:2020-06-08 Published:2020-12-10
  • Contact: LI Donghui,ZHANG Feng
  • Supported by:
    National Key Research and Development Program of China(2017YFC1601600);National"Ten Thou- sand Plan"Scientific and Technological Innovation Leading Talent Project (Feng ZHANG)

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摘要：

建立了QuEChERS结合超高效液相色谱-四极杆静电场轨道离子阱质谱测定鱼肉中15种降血脂药残留量的方法。样品前处理采用优化的QuEChERS法，通过响应面法优化了吸附剂材料乙二胺-N-丙基硅烷（PSA）（20、60、100、140和180 mg）、C18（40、100、160、220和280 mg）及乙酸钠（0.2、0.6、1.0、1.4和1.8 g）的用量。液相色谱采用XBridge-C18色谱柱（100 mm×2.1 mm，3.5 μm），以乙腈-0.1%（v/v）甲酸水溶液（含1.5 mmol/L乙酸铵）为流动相进行梯度洗脱，采用加热电喷雾电离（HESI）源，在正、负离子同时检测模式下以全扫描（full-MS）和二级质谱扫描（dd-MS2）方式对目标物进行定性和定量分析。15种降血脂药在各自范围内线性关系良好，相关系数（R2）大于0.99；检出限（LOD，S/N=3）和定量限（LOQ，S/N=10）分别为0.2~1.0 μg/kg和0.3~3.1 μg/kg；鱼肉样品中15种降血脂药在LOQ、2倍LOQ和10倍LOQ水平下的加标回收率为76.4%~116.0%，日内日精密度为1.0%~7.9%，日间精密度为1.7%~18.4%。该法前处理简单，灵敏度高，回收率高，适用于鱼肉中降血脂药的检测。

关键词: 超高效液相色谱, 四极杆/静电场轨道离子阱质谱法, QuEChERS, 降血脂药, 鱼肉

Abstract:

An analytical method was established for the determination of 15 lipid regulators in fish meat by QuEChERS combined with ultra performance liquid chromatography-quadrupole/electrostatic field orbitrap mass spectrometry (UPLC-Q/Orbitrap-MS). The samples were purified by optimized QuEChERS methods. The amounts of the adsorbent materials (primary secondary amine (PSA) (20, 60, 100, 140 and 180 mg), C18 (40, 100, 160, 220 and 280 mg) and sodium acetate (0.2, 0.6, 1.0, 1.4 and 1.8 g)) were optimized by the response surface method to obtain the best purification effect. The target compounds were separated on an XBridge-C18 column (100 mm×2.1 mm, 3.5 μm) using acetonitrile-0.1% (v/v) formic acid aqueous solution (containing 1.5 mmol/L ammonium acetate) as the mobile phases by a gradient elution program. Qualitative and quantitative analysis of the target compounds were performed in the full scan and secondary mass spectrometry scan (dd-MS2) modes with positive and negative ionization. The target compounds showed good linear relationships in their respective ranges, with correlation coefficients (R2) greater than 0.99. The limits of detection (LOD, S/N=3) and limits of quantification (LOQ, S/N=10) were in the range of 0.2-1.0 μg/kg and 0.3-3.1 μg/kg, respectively. The average recoveries were 76.4%-116.0% at LOQ, 2-fold LOQ, and 10-fold LOQ levels. The intra-day relative standard deviations (RSDs) were 1.0%-7.9%, and the inter-day RSDs were 1.7%-18.4%. The method is simple, sensitive and accurate, and it is suitable for the determination and quantification of lipid regulators in fish meat.

Key words: ultra performance liquid chromatography (UPLC), quadrupole/electrostatic field orbitrap mass spectrometry (Q/Orbitrap-MS), QuEChERS, lipid regulators, fish meat