超高效液相色谱质谱联用法测定牛肺表面活性提取物中残留四环素类药物  

Determination of Multi-Residues of Tetracycline in Calf Pulmonary Surfactant Extract by UPLC-MS/MS Method

作　　者：李珉 侯金凤 王成刚[1] 李文东[1] 车宝泉[1] 王俊秋[1] LI Min;HOU Jin-feng;WANG Cheng-gang;LI Wen-dong;CHE Bao-quan;WANG Jun-qiu(Beijing Institute for Drug Control, Beijing Municipal Key Laboratory for Analysis of Traditional Chinese Medicines and Biological Evaluation, Beijing 102206, China)

机构地区：[1]北京市药品检验所中药成分分析与生物评价北京市重点实验室,北京102206

出　　处：《中国药学杂志》2018年第8期632-638,共7页Chinese Pharmaceutical Journal

摘　　要：目的建立测定牛肺表面活性提取物中多种四环素类抗生素残留的方法。方法采用UPLC-MS/MS方法,以Waters HSS T3色谱柱(2.1 mm×100 mm,1.8μm)为固定相,分别以含0.1%甲酸的乙腈溶液和0.1%甲酸的水溶液为流动相A和流动相B,梯度洗脱,流速0.3 m L·min^(-1),柱温30℃,进样量1μL。结果该方法能同时测定四环素、金霉素、土霉素、多西环素、美他环素、米诺环素、β-多西环素、差向四环素、差向金霉素、脱水四环素和脱水差向四环素等11种抗生素。各化合物线性范围、灵敏度、精密度、回收率均满足分析要求。在牛肺表面活性提取物中可检出土霉素和四环素,其中土霉素残留量约为0.03 mg·kg^(-1),四环素则未达到定量限(0.006 mg·kg^(-1))。结论该方法可作为检测牛肺表面活性提取物中四环素类抗生素残留的方法。OBJECTIVE To establish a method for the determination of various tetracycline antibiotics residues in calf pulmonary surfactant extract.METHODS UPLC-MS/MS method was adopted with,Waters HSS T3 column（2.1 mm×100 mm,1.8 μm）as solid phase.A acetonitrile solution（containing 0.1% formic acid）and aqueous solution（containing 0.1% formic acid）were used as mobile phase A and mobile phase B,respectively.Gradient elution was conducted at,the flow rate of 0.3 mL·min-1,the column temperature was maintained at 30 ℃,and the injection volume was 1 μL.RESULTS This method can simultaneously determine 11 antibiotics,including tetracycline,chlortetracycline,oxytetracycline,doxycycline,metacycline,minocycline,β-doxycycline,epi-tetracycline,epi-chlortetracycline,anhydrotetracycline,and epi-anhydrotetracycline.The linear range,sensitivity,precision and recoveries of each compound meet the analytical requirements.Tetracycline and oxytetracycline were detected in the calf pulmonary surfactant extract samples.The amount of oxytetracycline residues was about 0.03 mg·kg-1,and the tetracycline did not reach the limit of quantitation（0.006 mg·kg-1）.CONCLUSION The method can be used for detecting tetracycline antibiotic residues in calf pulmonary surfactant extract.

关 键 词：四环素类 抗生素 残留 超高效液相色谱串联质谱法 牛肺表面活性提取物 固相萃取 

分 类 号：R917[医药卫生—药物分析学]