注射用阿莫西林钠/克拉维酸钾中两组分成盐率的分析

Analysis of the salt-forming rate of two components in amoxicillin sodium and clavulanate potassium for injection

目的建立离子色谱法同时测定注射用阿莫西林钠/克拉维酸钾中钠离子与钾离子的含量,通过计算其成盐率,对不同企业样品的成盐工艺进行评价。方法采用IonPacCS12A阳离子交换色谱柱(4mm×250mm)和IonPac CG12A保护柱(4mm×50m m),检测器为电导检测器,抑制器电流为20mA,以6.7mmol/L甲烷磺酸溶液为淋洗液,流速为1.0 mL/min。结果钠离子浓度在6.01~18.04μg/mL范围内与峰面积呈良好的线性关系(r=0.9999,n=5);平均回收率为100.4%(RSD=0.4%,n=9);钾离子浓度在3.33~9.98μg/mL范围内与峰面积呈良好的线性关系(r=0.9998,n=5);平均回收率为100.2%(RSD=0.5%,n=9)。测定了37批注射用阿莫西林钠/克拉维酸钾中钠和钾的含量,其成盐率分别为1.00~1.13和0.94~1.05。结论本方法可用于注射用阿莫西林钠/克拉维酸钾中钠离子与钾离子的含量测定,各企业样品成盐情况较好,但需关注成盐剂的残留。

Objective This research established an ion chromatographic method for simultaneous determination of sodium and potassium ions in amoxicillin sodium and clavulanate potassium for injection.According to the saltforming rate,the salt-forming processes of different enterprises were evaluated.Methods A cation exchange chromatography column of IonPac CS-12A(4 mm×250 mm)and a protection column of IonPac CG-12A(4 mm×50 mm)were used.The detector was a suppressed conductivity detector,and the suppressor current was 20 mA.An isocratic eluent of 6.7 mmol/L of methane sulfonic acid(MSA)solution was chosen as the mobile phase,with a flow rate of 1.0 mL/min.Results The linear correlation of sodium ions was good within the range of 6.01~18.04μg/mL(r=0.9999,n=5).The average recovery was 100.4%(RSD=0.4%,n=9).The linear correlation of potassium ions was good within the range of 3.33~9.98μg/mL(r=0.9998,n=5).The average recovery was 100.2%(RSD=0.5%,n=9).The content of sodium and potassium ions in 37 batches of amoxicillin sodium and clavulanate potassium for injection were determined,with salt-forming rates ranging from 1.00 to 1.13 and 0.94 to 1.05,respectively.Conclusions This method could be used for the determination of sodium and potassium ions in amoxicillin sodium and clavulanate potassium for injection.The salt-forming rate of samples from various enterprises was promising,but attention should be paid to the residue of salt-forming agents.