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首页> 美国卫生研究院文献>The Journal of Automatic Chemistry >Implementation and Validation of an Analytical Method for Lincomycin Determination in Feathers and Edible Tissues of Broiler Chickens by Liquid Chromatography Tandem Mass Spectrometry
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Implementation and Validation of an Analytical Method for Lincomycin Determination in Feathers and Edible Tissues of Broiler Chickens by Liquid Chromatography Tandem Mass Spectrometry

机译：液相色谱串联质谱法测定肉鸡和食用组织中林可霉素的分析方法的实现与验证

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Recent studies have detected different antimicrobial residues in broiler chicken feathers, where they persisted for longer periods of time and at greater concentrations than in edible tissues. However, until today, lincomycin behaviour in this nonedible tissue has not been assessed yet. Considering this, an analytical methodology to detect and quantify this antibiotic concentration in feathers, muscle, and liver tissues from broiler chickens was implemented and in-house validated. The methodology will allow the determination of the bioaccumulation of this highly persistent antibiotic in feathers of treated birds. For this purpose, 98% lincomycin and 95% lincomycin D3 standards were used. Methanol was selected as the extraction solvent, and Chromabond® Florisil® cartridges were used for the clean-up stage. The separation of analytes was performed through the analytical column SunFire C18 with a running time of 4 minutes, and the instrumental analysis was performed through an LC-MS/MS, with a liquid chromatograph Agilent® 1290 Infinity, coupled to an AB SCIEX® API 5500 mass spectrometer. An internal protocol for an in-house validation was designed based on recommendations from Commission Decision 2002/657/EC and the Guidance document on the estimation of limit of detection and limit of quantification for measurements in the field of contaminants in feed and food. The average retention time for lincomycin was 2.255 min (for quantifier ion, 126.0). The calibration curves showed a coefficient of determination (r2) greater than 0.99 for all matrices, while recovery levels ranged between 98% and 101%. The limit of detection (LOD) calculated was of 19, 22, and 10 μg·kg−1, and the limit of quantification (LOQ) was of 62, 73, and 34 μg·kg−1 in feathers, muscle, and liver, respectively. This method detects lincomycin in the studied matrices, confidently and accurately, as it is required for designing analytical studies of drug residues in edible and nonedible tissues, such as feathers.
机译：最近的研究已经在肉鸡的羽毛中检测到了不同的抗菌残留物，这些残留物比可食用组织中的残留时间更长，浓度更高。然而，直到今天，尚未评估林可霉素在该非食用组织中的行为。考虑到这一点，实施了一种分析方法来检测和定量肉鸡的羽毛，肌肉和肝组织中的这种抗生素浓度，并在内部进行了验证。该方法将可以确定这种高度持久性抗生素在经过处理的鸟类羽毛中的生物蓄积性。为此，使用了98％的林可霉素和95％的林可霉素D3标准品。选择甲醇作为萃取溶剂，并使用Chromabond®Florisil®小柱进行净化。通过运行时间为4分钟的分析柱SunFire C18进行分析物的分离，并通过液相色谱仪LC-MS / MS和结合了ABSCIEX®API的Agilent 1290 Infinity液相色谱仪进行仪器分析5500质谱仪。根据委员会第2002/657 / EC号决定和关于饲料和食品污染物领域中检测限的估计和定量限的估计的指导文件的建议，设计了内部验证的内部协议。林可霉素的平均保留时间为2.255 min（定量离子为126.0）。校正曲线显示，所有基质的测定系数（r 2 ）均大于0.99，而回收率介于98％和101％之间。计算的检出限（LOD）为19、22和10μg·kg -1 ，定量限（LOQ）为62、73和34μg·kg −1 分别位于羽毛，肌肉和肝脏中。该方法可用于设计可食用和不可食用组织（例如羽毛）中药物残留的分析研究，从而可以自信而准确地检测所研究基质中的林可霉素。

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