基于降解反应的共振散射光谱法测定头孢哌酮钠含量  

Determination of Cefoperazone Sodium by Resonance Scattering Spectroscopy Based on Degradation Reaction

作　　者：李鑫雨 孙双姣 罗聪 李鑫 张林林 LI Xinyu;SUN Shuangjiao;LUO Cong;LI Xin;ZHANG Linlin(School of Pharmacy,Shaoyang University,Shaoyang 422000,China)

机构地区：[1]邵阳学院药学院,邵阳422000

出　　处：《理化检验（化学分册）》2020年第9期951-954,共4页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：湖南省大学生创新性实验计划项目(2017611);湖南省自科基金(2018JJ2363)。

摘　　要：在碱性和加热的条件下,头孢哌酮钠会降解为降解产物Ⅰ(R′SH)与降解产物Ⅱ(R″SH)两种巯基化合物。在pH为4.4时,R′SH可使Cu(Ⅱ)还原为Cu(Ⅰ),生成的Cu(Ⅰ)进一步与R″SH生成白色溶胶,导致体系产生共振散射效应,基于此建立了共振散射光谱法测定头孢哌酮含量的方法。优化试验条件如下:①氢氧化钠溶液浓度为0.20mol·L^-1;②头孢哌酮钠的降解时间为40min;③pH 4.4乙酸-乙酸钠缓冲溶液的用量为1.00mL;④5.00mmol·L^-1 Cu(Ⅱ)溶液用量为0.50mL;⑤反应时间为2min。头孢哌酮钠的质量浓度与反应体系共振散射强度变化量(ΔIRSS)在0.02~2.40mg·L^-1内呈线性关系,检出限(3s/k)为0.006 2mg·L^-1。方法直接用于针剂中头孢哌酮钠含量的测定,加标回收率为97.5%~103%,测定值的相对标准偏差(n=5)为2.0%~2.6%。Under the conditions of alkaline and heating,cefoperazone sodium could be degraded to two sulfhydryl compounds(R′SH and R″SH).At pH 4.4,Cu(Ⅱ)was reduced to Cu(Ⅰ)by R′SH and then generated leucosol with R″SH,which leaded to the resonance scattering signal(RSS)increase drastically.Based on this fact,a method of resonance scattering spectroscopy for determination of cefoperazone sodium was proposed.The optimized conditions found were as follows:① concentration of sodium hydroxide solution:0.20 mol·L^-1;② degradation time of cefoperazone sodium:40 min;③amount of HOAc-NaOAc buffer solution at pH 4.4:1.00 mL;④amount of 5.00 mmol·L^-1 Cu(Ⅱ):0.50 mL;⑤ time of reaction:2 min.Linear relationship was obtained between enhanced RSS intensity(ΔIRSS)and concentration of cefoperazone sodium in the range of 0.02 to 2.40 mg·L^-1,with detection limit(3 s/k)of 0.006 2 mg·L^-1.The proposed method was applied to the determination of cefoperazone sodium in injection,giving results of recovery in the range of 97.5%to 103%.Values of RSDs(n=5)found were in the range of 2.0% to 2.6%.

关 键 词：共振散射光谱法 头孢哌酮钠 降解反应 

分 类 号：O657.39[理学—分析化学]