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采用改良的QuEChERS萃取法结合液相色谱-轨道阱质谱联用技术对猪肉中的多种抗生素进行筛查。

Screening of multi-class antibiotics in pork meat by LC-Orbitrap-MS with modified QuEChERS extraction.

作者信息

Chen Qing, Pan Xiao-Dong, Huang Bai-Fen, Han Jian-Long, Zhou Biao

机构信息

Zhejiang Provincial Center for Disease Control and Prevention, Institute of Physical-Chemistry and Toxicity Room No. 401, Bin-Sheng Road No. 3399, Binjiang District Hangzhou 310051 China

出版信息

RSC Adv. 2019 Sep 6;9(48):28119-28125. doi: 10.1039/c9ra04853g. eCollection 2019 Sep 3.

Abstract

The quantification capability of high resolution mass spectrometry is of great interest to analysts. We described a method for analysis of multi-class antibiotics in pork meat by UPLC-quadrupole (Q)-Orbitrap-MS. The QuEChERS approach with a clean-up step using a sorbent of primary-secondary amine (PSA) and C18 was adopted for sample preparation, and 37 antibiotics including beta-lactams, tetracyclines, sulfonamides, fluoroquinolones and macrolides were analyzed. The Q-Orbitrap method showed high sensitivity with limits of detection (LODs) ranging from 0.8 μg kg to 2.9 μg kg. The method was further validated by intra and inter-day tests with fortified samples. Recovery (85-105.6%) and precision values (RSDs < 15%) for all analytes were obtained. The result indicates that UPLC-Q-Orbitrap-MS coupled with QuEChERS preparation can serve as a routine method for multi-class antibiotic analysis in pork meat.

摘要

高分辨率质谱的定量能力引起了分析人员的极大兴趣。我们描述了一种通过超高效液相色谱-四极杆(Q)-轨道阱质谱分析猪肉中多类抗生素的方法。采用了QuEChERS方法,使用伯仲胺(PSA)和C18吸附剂进行净化步骤来制备样品,并分析了37种抗生素,包括β-内酰胺类、四环素类、磺胺类、氟喹诺酮类和大环内酯类。Q-轨道阱方法显示出高灵敏度,检测限(LOD)范围为0.8 μg/kg至2.9 μg/kg。通过对加标样品进行日内和日间测试进一步验证了该方法。获得了所有分析物的回收率(85 - 105.6%)和精密度值(相对标准偏差<15%)。结果表明,超高效液相色谱-Q-轨道阱质谱结合QuEChERS制备方法可作为猪肉中多类抗生素分析的常规方法。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/1085/9071086/4fc4ccceefda/c9ra04853g-f1.jpg

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