A detection and confirmation strategy for screening of veterinary drugs in honey by liquid chromatography coupled quadrupole time-of-flight mass spectrometry†,Analytical Methods

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A detection and confirmation strategy for screening of veterinary drugs in honey by liquid chromatography coupled quadrupole time-of-flight mass spectrometry†
Analytical Methods ( IF 2.7 ) Pub Date : 2017-11-23 00:00:00 , DOI: 10.1039/c7ay02440a
Zhibin Wang _{1,

2,

3,

4,

5} , Yan Li _{1,

2,

3,

4,

5} , Qiaoying Chang _{1,

2,

3,

4,

5} , Jian Kang _{6,

7,

8} , Guo-Fang Pang _{1,

2,

3,

4,

5}

Affiliation

A strategy for the quantification and confirmation of 40 multi-class veterinary drugs in honey by QuEChERS (quick, easy, cheap, effective, rugged, and safe) combined with liquid chromatography coupled quadrupole time-of-flight mass spectrometry (LC-Q-TOF/MS) is described. The veterinary drugs examined belong to four classes: quinolones, sulfonamides, macrolides, and tetracyclines. Before analysis by LC-Q-TOF/MS, the sample was diluted with a solution of Na₂EDTA-McIlvaine buffer solution (0.1 M, pH = 4), extracted with 5% acetic acid in acetonitrile, and cleaned up with an NH₂ sorbent. The average recoveries for the majority of analytes (86.9%), based on matrix-matched external calibration curves, were between 70% and 120%, and there was no significant difference in the recoveries between different honey matrices. The repeatability and reproducibility of the method expressed as the RSDs were less than 20% for all analytes. The data acquired by LC-Q-TOF/MS were cross-referenced with an accurate mass database of veterinary drugs, and the suspected analytes were finally confirmed based on a full product ion library match. Compared with the low-resolution MS technique, obvious advantages were obtained in terms of confirmation and identification by LC-Q-TOF/MS. The applicability of the method was verified by applying it to 12 different honey samples, and ciprofloxacin residue (at 99.7 μg kg⁻¹) was detected in one sample.

中文翻译：

液相色谱-四极杆飞行时间质谱法检测蜂蜜中兽药的检测和确认策略†

通过QuEChERS（快速，简便，廉价，有效，坚固和安全）与液相色谱结合四极杆飞行时间质谱（LC-Q-描述了TOF / MS。检查的兽药分为四类：喹诺酮类，磺酰胺类，大环内酯类和四环素类。在通过LC-Q-TOF / MS分析之前，将样品用Na ₂ EDTA-MlIlvaine缓冲溶液（0.1 M，pH = 4）稀释，用5％乙腈的乙酸萃取，并用NH2净化_2个吸附剂。根据基质匹配的外部校准曲线，大多数分析物（86.9％）的平均回收率在70％至120％之间，并且不同蜂蜜基质之间的回收率没有显着差异。对于所有分析物，用RSD表示的方法的重复性和重现性均低于20％。通过LC-Q-TOF / MS获得的数据与准确的兽药质量数据库进行了交叉引用，最终根据完整的产品离子库匹配结果对可疑分析物进行了确认。与低分辨率质谱技术相比，LC-Q-TOF / MS在确认和鉴定方面获得了明显的优势。通过将该方法应用于12种不同的蜂蜜样品以及环丙沙星残留量（99.7μgkg ^-1时），验证了该方法的适用性。在一个样品中被检测到。

更新日期：2017-11-23

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