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Quantitative analysis of total methenolone in animal source food by liquid chromatography-tandem mass spectrometry.
Drug Testing and Analysis ( IF 2.6 ) Pub Date : 2020-08-27 , DOI: 10.1002/dta.2915 Junping Zheng 1, 2 , Cheng Ye 3 , Peng Wang 3 , Yang Liu 1 , Huabing Yang 2 , Hongtao Liu 2
Drug Testing and Analysis ( IF 2.6 ) Pub Date : 2020-08-27 , DOI: 10.1002/dta.2915 Junping Zheng 1, 2 , Cheng Ye 3 , Peng Wang 3 , Yang Liu 1 , Huabing Yang 2 , Hongtao Liu 2
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Methenolone, an anabolic androgenic steroid, has been applied to improve the quality and protein content of meat in animal husbandry. However, the usage of methenolone in sports is banned for its doping effects. Several methods have been reported to monitor the content of methenolone in serum and urine samples, but a highly sensitive detection system has not been developed for the determination of methenolone in animal source food due to its constituent complexity. In this study, a novel detection system was developed to quantify the contents of both free and conjugated methenolone in animal source food including pork, beef, mutton, milk, and eggs by using high‐performance liquid chromatography‐tandem mass spectrometry (HPLC‐MS/MS) coupled with delicate pretreatment procedures. The conjugated methenolone in the above food samples was released by dual enzyme digestion, and the total methenolone was extracted by 1% formic acid in acetonitrile, followed by the purification using a PRiME HLB column or QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) salt. The compound d3‐methyltestosterone was used as an internal standard to minimize matrix interference. Finally, a wide linear range (0.5–20 μg/kg), low limit of detection (LOD) (0.3 μg/kg), good precision (<7% relative standard deviation), and high recovery (>90%) were obtained in the study of method validation. In summary, this analytical method provides a practicable monitoring tool for the quantification of methenolone in animal source food.
中文翻译：
液相色谱-串联质谱法定量分析动物源性食品中的总美替诺龙。
美替诺龙是一种合成代谢雄激素类固醇，已被用于提高畜牧业肉类的质量和蛋白质含量。然而，美替诺龙因其兴奋剂效应而被禁止在运动中使用。已有多种方法用于监测血清和尿液样本中美替诺龙的含量，但由于其成分复杂，尚未开发出用于测定动物源性食品中美替诺龙的高灵敏度检测系统。本研究开发了一种新型检测系统，通过使用高效液相色谱-串联质谱 (HPLC-MS) 对包括猪肉、牛肉、羊肉、牛奶和鸡蛋在内的动物源食品中游离和结合美替诺龙的含量进行定量。 /MS) 加上精细的预处理程序。上述食品样品中的结合美替诺龙经双酶消化释放，总美替诺龙用1%甲酸乙腈溶液提取，然后用PRiME HLB柱或QuEChERS（Quick, Easy,Cheap, Effective, Rugged）纯化, 和安全) 盐。化合物 d3-甲基睾酮用作内标以尽量减少基质干扰。最后，获得了较宽的线性范围 (0.5–20 μg/kg)、低检测限 (LOD) (0.3 μg/kg)、良好的精密度（<7% 相对标准偏差）和高回收率（>90%）在方法验证的研究中。总之，该分析方法为动物源食品中美替诺龙的定量提供了一种切实可行的监测工具。
更新日期：2020-08-27
中文翻译：
液相色谱-串联质谱法定量分析动物源性食品中的总美替诺龙。
美替诺龙是一种合成代谢雄激素类固醇，已被用于提高畜牧业肉类的质量和蛋白质含量。然而，美替诺龙因其兴奋剂效应而被禁止在运动中使用。已有多种方法用于监测血清和尿液样本中美替诺龙的含量，但由于其成分复杂，尚未开发出用于测定动物源性食品中美替诺龙的高灵敏度检测系统。本研究开发了一种新型检测系统，通过使用高效液相色谱-串联质谱 (HPLC-MS) 对包括猪肉、牛肉、羊肉、牛奶和鸡蛋在内的动物源食品中游离和结合美替诺龙的含量进行定量。 /MS) 加上精细的预处理程序。上述食品样品中的结合美替诺龙经双酶消化释放，总美替诺龙用1%甲酸乙腈溶液提取，然后用PRiME HLB柱或QuEChERS（Quick, Easy,Cheap, Effective, Rugged）纯化, 和安全) 盐。化合物 d3-甲基睾酮用作内标以尽量减少基质干扰。最后，获得了较宽的线性范围 (0.5–20 μg/kg)、低检测限 (LOD) (0.3 μg/kg)、良好的精密度（<7% 相对标准偏差）和高回收率（>90%）在方法验证的研究中。总之，该分析方法为动物源食品中美替诺龙的定量提供了一种切实可行的监测工具。
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