HPLC-PDA法测定恩诺沙星注射液中非法添加乙酰甲喹和水杨酸
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摘要
建立了高效液相色谱法测定恩诺沙星注射液中非法添加乙酰甲喹、水杨酸含量的方法。试验采用十八烷基硅烷键合硅胶色谱柱,以0.025 moL/L磷酸溶液-乙腈(85∶15,V/V)为流动相,流速为1.0 m L/min,二极管阵列检测器进行全扫描和232 nm波长测定。结果表明乙酰甲喹在0.5～20μg/m L范围内线性良好,R~2=1.000,平均回收率为99.62%;水杨酸在1.0～50μg/m L范围内线性良好,R~2=1.000,平均回收率为99.51%;RSD在0.07%～3.44%之间。本方法准确、可靠、重现性好,可用于恩诺沙星注射液中非法添加乙酰甲喹、水杨酸的定性和定量检测。
A method was developed and validated for the content determination of maquindox and salicylic acid in enrofloxacin injection by HPLC. It was tested with C18 column,using phosphorous acid solution-methanol( 85 ∶ 15,V/V) as the mobile phase. The extract wave length was 232 nm from full scan. Results showed that the calibration curve of maquindox was good linear between the peak areas and the concentrations of 0.5 ～ 20 μg/m L,the correlation coefficient( r) was 1.000 and the mean recovery was 99.62%; the calibration curve of salicylic acid was good linear between the peak areas and the concentrations of 1.0 ～ 50 μg/m L,the correlation coefficient( r) was 1.000 and the mean recovery was 99.51%; RSD was 0.07% ～ 3.44%. In conclusion,the method was accurate,reliable and reproducible,and provided a reliable way for detecting acetoquine and salicylic acid adulterated in enrofloxacin injection.
A method was developed and validated for the content determination of maquindox and salicylic acid in enrofloxacin injection by HPLC. It was tested with C18 column,using phosphorous acid solution-methanol( 85 ∶ 15,V/V) as the mobile phase. The extract wave length was 232 nm from full scan. Results showed that the calibration curve of maquindox was good linear between the peak areas and the concentrations of 0.5 ～ 20 μg/m L,the correlation coefficient( r) was 1.000 and the mean recovery was 99.62%; the calibration curve of salicylic acid was good linear between the peak areas and the concentrations of 1.0 ～ 50 μg/m L,the correlation coefficient( r) was 1.000 and the mean recovery was 99.51%; RSD was 0.07% ～ 3.44%. In conclusion,the method was accurate,reliable and reproducible,and provided a reliable way for detecting acetoquine and salicylic acid adulterated in enrofloxacin injection.
引文
[1]中国兽药典委员会.中华人民共和国兽药典2015年版(一部)[S].Commission of Chinese Veterinary Pharmacopoeia. Veterinary Pharmacopoeia of the People's Republic of China(the first volume of 2015 edition)[S].
[2]刘桂兰,夏雪林,仝玉慧,等.乙酰甲喹性质、毒性与替代药物[J].中国兽药杂志,2011,45(8):46-49.Liu G L,Xia X L,Tong Y H,et al. Character,Toxin and Substitution of Maquindox[J]. Chinese Journal of Veterinary Drug,2011,45(8):46-49.
[3]张志琴,司军强,呼海燕,等.水杨酸类药物的镇痛作用及其机制研究进展[J].石河子大学学报(自然科学版),2003,7(4):341-343.Zhang Zh Q,Si J Q,Hu H Y,et al. Progress of Analgesic Effect and Mechanism of Salicylates[J]. Journal of Shihezi University(Natural Science),2003,7(4):341-343.
[4]农业部.中华人民共和国农业部公告2508号[S].Ministry of Agriculture. No. 2508 Bulletin of the Ministry of Agriculture of the Pepole's Republic of China[S].
[5]李慧素,杜红鸽,吴宁鹏,等. HPLC-PDA法测定兽药中非法添加四种解热镇痛抗炎类药物[J].中国兽药杂志,2014,48(10):36-43.Li H S,Du H G,Wu N P,et al. Determination of Four Kinds of Illegal Additives Antipyretic-analgesic and Anti-inflammatory Drugs in Veterinary Drugs by HPLC-PDA[J].Chinese Journal of Veterinary Drug,2014,48(10):36-43.
[2]刘桂兰,夏雪林,仝玉慧,等.乙酰甲喹性质、毒性与替代药物[J].中国兽药杂志,2011,45(8):46-49.Liu G L,Xia X L,Tong Y H,et al. Character,Toxin and Substitution of Maquindox[J]. Chinese Journal of Veterinary Drug,2011,45(8):46-49.
[3]张志琴,司军强,呼海燕,等.水杨酸类药物的镇痛作用及其机制研究进展[J].石河子大学学报(自然科学版),2003,7(4):341-343.Zhang Zh Q,Si J Q,Hu H Y,et al. Progress of Analgesic Effect and Mechanism of Salicylates[J]. Journal of Shihezi University(Natural Science),2003,7(4):341-343.
[4]农业部.中华人民共和国农业部公告2508号[S].Ministry of Agriculture. No. 2508 Bulletin of the Ministry of Agriculture of the Pepole's Republic of China[S].
[5]李慧素,杜红鸽,吴宁鹏,等. HPLC-PDA法测定兽药中非法添加四种解热镇痛抗炎类药物[J].中国兽药杂志,2014,48(10):36-43.Li H S,Du H G,Wu N P,et al. Determination of Four Kinds of Illegal Additives Antipyretic-analgesic and Anti-inflammatory Drugs in Veterinary Drugs by HPLC-PDA[J].Chinese Journal of Veterinary Drug,2014,48(10):36-43.