A high-accuracy screening method of 44 cephalosporins in meat using liquid chromatography quadrupole-orbitrap hybrid mass spectrometry,Analytical Methods

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A high-accuracy screening method of 44 cephalosporins in meat using liquid chromatography quadrupole-orbitrap hybrid mass spectrometry
Analytical Methods ( IF 2.7 ) Pub Date : 2017-10-30 00:00:00 , DOI: 10.1039/c7ay01903c
Yun-He Hong _{1,

2,

3,

4,

5} , Xiu-Li Xu _{1,

2,

3} , Wei-Qing Li _{1,

2,

3} , Bo-Zhou Xu _{1,

2,

3} , Han-Qiu Wu _{1,

2,

3} , Yan Cheng _{1,

2,

3} , Hong Chen _{1,

2,

3} , Bao-Shan Zhang _{3,

4,

5} , Feng Zhang _{1,

2,

3}

Affiliation

In this study, we report the development of a screening method for highly accurate and sensitive analysis of 44 cephalosporins in 4 representative meats (pork, beef, chicken, and mutton). The approach is based on liquid chromatography quadrupole-orbitrap hybrid high resolution mass spectrometry (LC-Q-Orbitrap, HRMS). Highly accurate identification markers of cephalosporins were obtained to have a tool for the detection of non-target or even unknown cephalosporins. Optimal chromatographic separation was studied, and Ascentis C8 column was chosen after comparing several different column materials and mobile phases. A simple sample treatment method consisting of extraction with a mixture of acetonitrile and water followed by solid-phase extraction (SPE) with a PRiME HLB cartridge was developed. The methodology was validated in accordance with the Commission Decision 2002/657/EC by evaluating the following required parameters: linearity, accuracy, repeatability, decision limit (CCα), and detection capability (CCβ). For the matrices studied herein, the recovery rates ranged from 69.2% to 129.0% with the inter- and intra-day variability under 15%. The CCα and CCβ were determined according to maximum residue limit (MRL) or minimum required performance limit (MRPL) when established. The method has been successfully applied to meat samples purchased from the local market, and ceftazidime, which has not yet been considered in the current legislation all over the world, has been found in one of these samples.

中文翻译：

液相色谱-四极杆-轨道阱混合质谱法对肉类中44种头孢菌素的高精度筛选方法

在这项研究中，我们报告了一种筛查方法的发展，该方法可对4种代表性肉类（猪肉，牛肉，鸡肉和羊肉）中的44种头孢菌素进行高度准确和灵敏的分析。该方法基于液相色谱四极杆-Orbitrap混合高分辨率质谱（LC-Q-Orbitrap，HRMS）。获得了高精度的头孢菌素识别标记，以具有检测非靶标甚至未知头孢菌素的工具。研究了最佳的色谱分离效果，在比较了几种不同的色谱柱材料和流动相之后，选择了Ascentis C8色谱柱。开发了一种简单的样品处理方法，包括用乙腈和水的混合物萃取，然后用PRiME HLB柱进行固相萃取（SPE）。通过评估以下必需参数，根据委员会决定2002/657 / EC对方法进行了验证：线性，准确性，可重复性，决策极限（CCα）和检测能力（CCβ）。对于本文研究的基质，当日间和日内变异度低于15％时，回收率范围为69.2％至129.0％。建立时，根据最大残留限量（MRL）或最低要求的性能限量（MRPL）确定CCα和CCβ。该方法已成功应用于从当地市场购买的肉类样品，并且在其中一种样品中发现了头孢他啶，目前尚未在世界范围内的立法中予以考虑。和检测能力（CCβ）。对于本文研究的基质，当日间和日内变异度低于15％时，回收率范围为69.2％至129.0％。建立时，根据最大残留限量（MRL）或最低要求的性能限量（MRPL）确定CCα和CCβ。该方法已成功应用于从当地市场购买的肉类样品，并且在其中一种样品中发现了头孢他啶，目前尚未在世界范围内的立法中予以考虑。和检测能力（CCβ）。对于本文研究的基质，当日间和日内变异度低于15％时，回收率范围为69.2％至129.0％。建立时，根据最大残留限量（MRL）或最低要求的性能限量（MRPL）确定CCα和CCβ。该方法已成功应用于从当地市场购买的肉类样品，并且在其中一种样品中发现了头孢他啶，目前尚未在世界范围内的立法中予以考虑。

更新日期：2017-11-13

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