Tsou Tai-Li, Lee Chiu-Wey, Wang Hsian-Jenn, Cheng Ya-Chung, Liu Yu-Tien, Chen Su-Hwei
Kaohsiung Medical University, College of Pharmacy, Faculty of Pharmacy, Kaohsiung, Taiwan.
J AOAC Int. 2009 Jul-Aug;92(4):1089-94.
A new HPLC method has been developed and validated for the simultaneous determination of ticarcillin (TIC) and clavulanic acid (CA) in pharmaceutical formulations. The HPLC separation was achieved on a beta-cyclodextrin column (Cyclobond I, 250 x 4.6 mm, 5 microm) with methanol-16 mM pH 6.0 ammonium acetate buffer (50 + 50, v/v) mobile phase at a flow rate of 0.8 mL/min. Detection was at 220 nm. Validation of the method was performed by evaluating specificity, robustness, accuracy, and precision. The calibration curves were linear in the range of 1-100 microg/mL for CA and 2-200 microg/mL for TIC. The LOQs based on the standard regression lines were 0.42 and 1.42 microg/mL for CA and TIC, respectively, and the LOD were 0.14 and 0.47 microg/mL, respectively. Total recoveries of synthetic mixtures (CA:TIC = 1:10, 1:15, and 1:30) were 99.25-100.99% for CA and 99.54-100.82% for TIC. Compared with the U.S. Pharmacopeia method, the proposed method has the advantage of a relatively low flow rate and short analysis time. The proposed method was successfully applied for the simultaneous determination of these two drugs in sterilized H20 and 5% dextrose injection solutions.
已开发并验证了一种用于同时测定药物制剂中替卡西林（TIC）和克拉维酸（CA）的高效液相色谱新方法。高效液相色谱分离在β - 环糊精柱（Cyclobond I，250×4.6 mm，5μm）上进行，流动相为甲醇 - 16 mM pH 6.0醋酸铵缓冲液（50 + 50，v/v），流速为0.8 mL/min。检测波长为220 nm。通过评估特异性、稳健性、准确性和精密度对该方法进行验证。校准曲线在CA浓度为1 - 100μg/mL和TIC浓度为2 - 200μg/mL范围内呈线性。基于标准回归线的定量限（LOQ），CA和TIC分别为0.42和1.42μg/mL，检测限（LOD）分别为0.14和0.47μg/mL。合成混合物（CA:TIC = 1:10、1:15和1:30）中CA的总回收率为99.25 - 100.99%，TIC的总回收率为99.54 - 100.82%。与美国药典方法相比，该方法具有流速相对较低和分析时间短的优点。该方法已成功应用于同时测定灭菌注射用水和5%葡萄糖注射液中这两种药物的含量。
