El Hawari Khaled, Al Iskandarani Mohamad, Mompelat Sophie, Hurtaud-Pessel Dominique, Verdon Eric
CNRSL, Lebanese Atomic Energy Commission (LAEC), Laboratory for Analysis of Organic Compounds (LAOC), Airport Road, PO Box 11-8281, Beirut, Lebanon.
French Agency for Safety of Food, Environment and Occupational Health, Laboratory of Fougères, French National and European Union Reference Laboratory for Residues of Antimicrobial Veterinary Medicinal Products in Food from Animal Origin, 10B rue Claude Bourgelat, Bioagropolis, Javené, F-35306, Fougères, France.
Rapid Commun Mass Spectrom. 2017 Jul 15;31(13):1103-1110. doi: 10.1002/rcm.7899.
This paper investigates the validity of the transfer of a liquid chromatography/tandem mass spectrometry (LC/MS/MS) method for the determination of veterinary medicinal products in honey and compares it with an LC/linear ion trap/Orbitrap mass spectrometry method. A descriptive statistical approach was used in order to assess whether such a transfer would succeed or fail. This approach is based on the simultaneous evaluation of the trueness and of the intermediate precision for each compound at a 95% interval of confidence of both analytical techniques.
Two grams of honey were placed in a centrifuge tube and diluted with 2.5 mL of ultra-pure water and 2.5 mL of acidified methanol with hydrochloric acid at 2 mol.mL . The extract was purified with 50 mg of primary secondary amine and then analyzed using LC/MS/MS in multiple reaction monitoring (MRM) mode and LC/orbitrap high-resolution mass spectrometry in full scan mode. Both analytical techniques were compared by using the descriptive statistical approach for the determination of antimicrobial residues in honey.
The transfer of the method showed that the Orbitrap system provides the same accurate analytical results compared with the LC/MS/MS method except for 4-epitetracycline, anhydroerythromycin A, erythromycin A enol ether, and dihydrostreptomycin. Furthermore, the LC/LTQ-Orbitrap system is capable of successfully competing with the LC/MS/MS method by additional provision of high mass resolution and mass accuracy even though it shows less sensitivity compared with the LC/MS/MS instrument. CCα levels for most analytes were 1.3 times higher by LC/MS/MS than those observed by LC/LTQ-Orbitrap. The method was assessed in terms of relative bias through analysis of a reference material provided by FAPAS (Food Analysis Performance and Assessment Scheme) and also through the control of several contaminated honey samples from local Lebanese markets. Satisfactory relative bias was below 22% except for tetracycline found in one sample that showed a higher bias at 29%.
The LC/LTQ-Orbitrap method offers adequate performance in comparison with previously validated method on a LC/MS/MS system resulting in acceptance of the transfer of the method from LC/MS/MS to LC/LTQ-Orbitrap. Copyright © 2017 John Wiley & Sons, Ltd.
本文研究了液相色谱/串联质谱法（LC/MS/MS）测定蜂蜜中兽药产品方法转移的有效性，并将其与液相色谱/线性离子阱/轨道阱质谱法进行比较。采用描述性统计方法来评估这种方法转移是否成功。该方法基于在两种分析技术95%置信区间内对每种化合物的准确性和中间精密度进行同时评估。
将2克蜂蜜置于离心管中，用2.5毫升超纯水和2.5毫升含2摩尔/毫升盐酸的酸化甲醇稀释。提取物用50毫克伯仲胺净化，然后采用多反应监测（MRM）模式的LC/MS/MS和全扫描模式的LC/轨道阱高分辨率质谱进行分析。通过使用描述性统计方法测定蜂蜜中的抗菌残留，对两种分析技术进行比较。
方法转移表明，除4-表四环素、脱水红霉素A、红霉素A烯醇醚和二氢链霉素外，轨道阱系统与LC/MS/MS方法相比提供了相同的准确分析结果。此外，尽管LC/LTQ-轨道阱系统与LC/MS/MS仪器相比灵敏度较低，但通过额外提供高质量分辨率和质量准确度，它能够成功与LC/MS/MS方法竞争。大多数分析物的CCα水平通过LC/MS/MS比通过LC/LTQ-轨道阱观察到的高1.3倍。通过分析由FAPAS（食品分析性能和评估计划）提供的参考物质以及通过控制来自黎巴嫩当地市场的几个受污染蜂蜜样品，对该方法进行了相对偏差评估。除了在一个样品中发现的四环素偏差较高为29%外，令人满意的相对偏差低于22%。
与先前在LC/MS/MS系统上验证的方法相比，LC/LTQ-轨道阱方法具有足够的性能，从而使得该方法从LC/MS/MS转移到LC/LTQ-轨道阱被接受。版权所有© 2017约翰威立父子有限公司。
