液相色谱串联质谱法测定海鲈鱼中土霉素 四环素 金霉素 强力霉素含量的分析

Determination of Oxytetracycline,Tetracycline,Chlortetracycline,Doxycycline in Sea Perch Aureomycin by LC/MS/MS

研究建立海鲈鱼中四环素族的液相色谱/串联质谱（LC/MS/MS）方法。海鲈鱼样品经制样,1%高氯酸溶液提取土霉素、四环素、金霉素、强力霉素,固相萃取装置（SPE）净化,氮气吹干后用甲醇复溶。以Welch Materials Ultimate XD-C8色谱分离柱,乙腈-甲醇混合溶液、0.1%甲酸水溶液梯度洗脱,使用电喷雾三重四极杆串联质谱的多重反应监测模式（Multiple Reaction Monitoring,MRM）测定,以校准曲线法进行定量。所建立的液相色谱串联质谱法（LC/MS/MS）对于分析海鲈鱼中土霉素、四环素、金霉素、强力霉素的批内、批间RSD分别为0.12%-0.86%,0.10%-0.37%,回收率为91.7%-95.3%。

A measurement method for tetracyelines in sea perch involving LCMS/MS has been developed. The tetracyclines are extracted from sea perch using 1% perchloric acid and cleaned by solid-phase extractions prior to reversed-phase LC/MS/MS determination. Separation is performed on a Welch Materials Ultimate XB-C8 column using gradient elution with acetonitrile - methanol mixed solution and 0.1% formic acid. An agilent tandem mass spectrometer equipped with an electrospmy ionization source operated in multiple reaction monitoring （MRM） mode is utilized, and the results of determination are calculated from the calibration curve. The results of the LC/MS/MS method for the analysis of oxytetracycline, tetracycline, chlortetracycline, doxycycline in sea perch samples are as follows, the within-run RSD ranged from 0.12% to 0.86% , between-run RSD ranged from 0.10% to 0.37% and recoveries ranged between 91.7%-95.3%.