鸡组织中泰拉霉素残留的高效液相色谱-串联质谱法检测

Determination of Tulathromycin residues in chicken using liquid chromatography-tandem mass spectrometry

【目的】建立鸡血浆、肌肉、肝脏、肾脏中泰拉霉素残留的高效液相色谱串联质谱（HPLC-MS／MS）检测方法。【方法】制备鸡血浆、肌肉、肝脏、肾脏泰拉霉素加标样品，经乙腈提取，SCX固相萃取小柱净化后，40℃氮气吹干，用乙腈-1mL／L甲酸水溶液（4g积比为1：1）定容，LunaC18（2）色谱柱分离，以乙腈-1ML/L甲酸水溶液（体积比为90：10）为流动相进行梯度洗脱，通过质谱分析进行外标法定量，再通过试验确定HPLC—MS／MS的检出限和定量限，并对血浆和肌肉、肝脏、。肾脏分别进行10，20，50μg／L和10,20,50μg／kg3个水平的泰拉霉素添加回收试验。【结果】在5-200μg／L血浆样品和5-200μg／kg肌肉、肝脏、肾脏样品中，泰拉霉素含量与峰面积呈良好的线性关系（R〉0．99），血浆和肌肉、肝脏、肾脏样品中的泰拉霉素检出限依次为0.8μg／L和0.5，0.8，0.5μg／kg，定量限依次为2.0μg／L和1.0，2.0，1.0μg／kg。添加回收试验的平均回收率为80.3％-104.4％，日内相对标准偏差为5.0％-9.2％，日间相对标准偏差为5.2％-12.7％。【结论】HPLC-MS／MS方法简便、快速、准确，可用于鸡组织中泰拉霉素药物残留的确证和定量检测。

[Objective] An analytical method based on liquid chromatography tandem mass spectrome- try was developed for the determination of Tulathromycin residues in chicken tissues. [Method] Samples were extracted with acetonitrile and cleaned-up SCX cartridge. The Tulathromycin were separated with lu- na C18 column by a gradient elution program with 1 mL/L acetonitrile and 1 mL/L formic acid-water as the mobile phase. The identification of Tulathromycin was carried out by positive electrospray ionization （ESI＋） in multiple-reaction monitoring （MRM） mode. The quantitation was performed by the external standard method. Add and recovery experiment was also conducted with different Tulathromycin levels for plasma,muscle,liver and kidney. [Result] There was a good linear relationship between Tara kanamycin concentration and peak area （R〉0.99） in plasma （5-200 μg/L） and muscle, liver, and kidney （5-200 μg/kg）. Recovery rates were 80.3% to 104.4% at three spiked levels of 10,20,50 μg/kg and the relative standard deviations （RSDs） were 5.0%-9.2% for intra-day and 5.2%--12.7% for inter-day determina- tions. Limit of detection （LOD） and limit of quantitation （LOQ） of plasma, muscle, liver, and kidney sam- ples were 0.8 μg/L and 0.5,0.8,0.5 μg/kg,and 2.0 μg/L and 1.0,2.0,1.0 μg/kg,respectively. [Conclu- sion] The established method was simple, rapid,accurate and suitable for quantitative determination and confirmation of tulathromycin in real samples.