UPLC-PDA法同时测定兽药粉剂中非法添加五种头孢类药物

Simultaneous determination of five kinds of cephalosporins illegally added in veterinary medicine powder by UPLC-PDA method

为了建立兽药氟苯尼考可溶性粉、阿莫西林可溶性粉中非法添加头孢类药物头孢曲松、头孢噻肟、头孢呋辛、头孢西丁、头孢哌酮的检验方法,试验采用超高效液相色谱-二极管阵列检测法,色谱条件为:Waters ACQUITYUPLCBEH C18色谱柱(2.1 mm×50 mm,1.7μm),流动相为含0.5%甲酸的乙腈溶液(A)和含0.5%甲酸的水溶液(B),流速为0.3 m L/min,梯度洗脱,二极管阵列检测器,波长采集范围为200~400 nm,记录色谱图波长为262 nm,柱温为25℃,进样量为10μL。结果表明:五种头孢类药物质量浓度在10.0~200.0 mg/L范围内与峰面积呈良好线性关系,相关系数(r)均大于0.999 2。在氟苯尼考可溶性粉中五种头孢类药物的平均回收率在97.6%~101.9%(n=9)之间,在阿莫西林可溶性粉中五种头孢类药物的平均回收率在97.7%~102.4%(n=9)之间。本方法准确、简便、快速,适用于兽药氟苯尼考可溶性粉、阿莫西林可溶性粉中非法添加头孢曲松、头孢噻肟、头孢呋辛、头孢西丁、头孢哌酮五种头孢类药物的检查。

To establish a method for the detection of cephalosporins of ceftriaxone, cefotaxime, cefuroxime , cefoxitin, cefoperazone illegally added in soluble powders of florfenieol and amoxicillin, an ultra performance liquid chromatography - diode array detection method was used in the test. The chromatographic conditions were as follows： Waters ACQUITY UPLC BEH C18 column （2.1 mm × 50 mm, 1.7 μm） , mobile phase containing 0.5% formic acid in acetonitrile（A） and 0.5% formic acid in water（B） , flow rate of 0.3 mL/min, gradient elution, diode - array detector, wavelength range of 200 -400 nm, recorded wavelength of 262 nm, column temperature of 25 ℃, injection volume of 10 μL. The results showed that there was a good linear relationship between the concentration of the five kinds of cephalosporins and peak area within the range of 10.0 to 200.0 mg/L, and the correlation coefficients （r） were more than 0. 999 2. The average recoveries of five kinds of eephalosporinsin in the soluble powder of florfenicol were 97.6% to 101.9% （ n = 9 ） and those in the soluble powder of amoxicillin were 97.7% to 102.4% （ n = 9 ）. The results indicate that this method is accurate, easy and rapid. It is suitable for the detection of ceftriaxone , cefotaxime , cefuroxime , cefoxitin , eefoperazone illegally added in soluble powders of florfenicol and amoxicillin.