Detection and confirmation of zilpaterol in equine hair using liquid chromatography–mass spectrometry,Drug Testing and Analysis

当前位置： X-MOL 学术 › Drug Test. Anal. › 论文详情

Our official English website, www.x-mol.net, welcomes your feedback! (Note: you will need to create a separate account there.)

Detection and confirmation of zilpaterol in equine hair using liquid chromatography–mass spectrometry
Drug Testing and Analysis ( IF 2.6 ) Pub Date : 2021-08-06 , DOI: 10.1002/dta.3138
Benjamin C Moeller _{1,

2} , Amel Clifford ₁ , Richard T Emery ₁ , Gwen Alarcio ₁ , Gianna Favro ₁ , Rick M Arthur ₃

Affiliation

Zilpaterol is a β₂-adrenergic agonist and a repartitioning agent that has a high potential for abuse in equine performance athletes. Analysis of zilpaterol in hair is an alternative sampling matrix that extends detection time periods beyond those found in urine or blood samples. Our laboratory has been screening for zilpaterol in hair for many years and recently detected and confirmed its presence in official samples. Accordingly, a liquid chromatography–mass spectrometry method was developed and validated to detect and confirm zilpaterol in equine hair. Briefly, equine hair was decontaminated, cut, and pulverized prior to disruption and liquid–liquid extraction in basic conditions. Following extraction, the sample was introduced to an Agilent 1260 HPLC and zilpaterol was separated using a reverse phase gradient with a total run time of 12.5 min. Following chromatographic separation, zilpaterol and its corresponding stable isotope labeled internal standard were introduced via positive mode electrospray ionization to a Thermo Q-Exactive Plus mass spectrometer and spectra collected using parallel reaction monitoring. The methodology was validated using in-house criteria including characterization of accuracy, precision, recovery, linear range, matrix effects, limit of detection, and limit of quantitation, and the method was found to be fit-for-purpose to confirm the presence of zilpaterol in equine hair. This methodology has been used to detect and confirm the presence of zilpaterol from out-of-competition hair samples submitted by regional racing authorities.

中文翻译：

液相色谱-质谱法检测和确认马毛中的齐帕特罗

齐帕特罗是一种_β2- 肾上腺素能激动剂和重新分配剂，在马表现运动员中具有很高的滥用潜力。头发中齐帕特罗的分析是另一种采样矩阵，可将检测时间延长到尿液或血液样本中发现的时间段之外。我们的实验室多年来一直在筛选头发中的齐帕特罗，最近在官方样本中检测并证实了它的存在。因此，开发并验证了一种液相色谱-质谱方法来检测和确认马毛中的齐帕特罗。简而言之，在基本条件下破坏和液-液萃取之前，对马毛进行去污、切割和粉碎。萃取后，将样品引入 Agilent 1260 HPLC 并使用反相梯度分离齐帕特罗，总运行时间为 12.5 分钟。色谱分离后，齐帕特罗及其相应的稳定同位素标记的内标通过正模式电喷雾电离引入 Thermo Q-Exactive Plus 质谱仪，并使用平行反应监测收集光谱。该方法使用内部标准进行了验证，包括准确度、精密度、回收率、线性范围、基质效应、检测限和定量限的表征，并且发现该方法适用于确认存在马毛中的齐帕特罗。该方法已用于检测和确认地区赛马当局提交的赛外头发样本中齐帕特罗的存在。通过正模式电喷雾电离将齐帕特罗及其相应的稳定同位素标记的内标引入 Thermo Q-Exactive Plus 质谱仪，并使用平行反应监测收集光谱。该方法使用内部标准进行了验证，包括准确度、精密度、回收率、线性范围、基质效应、检测限和定量限的表征，并且发现该方法适用于确认存在马毛中的齐帕特罗。该方法已用于检测和确认地区赛马当局提交的赛外头发样本中齐帕特罗的存在。通过正模式电喷雾电离将齐帕特罗及其相应的稳定同位素标记的内标引入 Thermo Q-Exactive Plus 质谱仪，并使用平行反应监测收集光谱。该方法使用内部标准进行了验证，包括准确度、精密度、回收率、线性范围、基质效应、检测限和定量限的表征，并且发现该方法适用于确认存在马毛中的齐帕特罗。该方法已用于检测和确认地区赛马当局提交的赛外头发样本中齐帕特罗的存在。该方法使用内部标准进行了验证，包括准确度、精密度、回收率、线性范围、基质效应、检测限和定量限的表征，并且发现该方法适用于确认存在马毛中的齐帕特罗。该方法已用于检测和确认地区赛马当局提交的赛外头发样本中齐帕特罗的存在。该方法使用内部标准进行了验证，包括准确度、精密度、回收率、线性范围、基质效应、检测限和定量限的表征，并且发现该方法适用于确认存在马毛中的齐帕特罗。该方法已用于检测和确认地区赛马当局提交的赛外头发样本中齐帕特罗的存在。

更新日期：2021-08-06

点击分享查看原文

点击收藏

阅读更多本刊最新论文本刊介绍/投稿指南11