HPLC法测定并比较药用级与非药用级苯甲酸钠的含量

摘要

OBJECTIVE:To establish a method to determine and compare the contents of sodium benzoate in medicinal(phar-maceutical excipients and active pharmaceutical ingredients) and non-medicinal (chemical reagents and food additives) grade. METHODS:HPLC was conducted for content determination,SPSS 18.0 software was adopted to compare the results. The column was Purospher STAR LP RP-18 endcapped with mobile phase of acetotrile-0.02% formic acid(adjusted pH to 4.0 with aqua ammo-nia)(30∶70,V/V)at a flow rate was 1.0 ml/min,the detection wavelength was 230 nm,column temperature was 35 ℃,and vol-ume injection was 20 μl. RESULTS:The linear range of sodium benzoate was 10.5-525.3 μg/ml(r=0.999 9);RSDs of precision, stability,reproducibility and durability tests were lower than 0.5%;recovery was 99.38%-101.26%(RSD=0.56%,n=9). The av-erage contents of sodium benzoate in medicinal and non-medicinal grade were between 99.400%-99.875%,but the average content of non-medicinal grade is lower than the medical grade. CONCLUSIONS:The method is accurate and simple with high specificity and good reproducibility,and can be used to determine and compare the content of sodium benzoate in medicinal and non-medici-nal grade.%目的：建立测定并比较药用级（药用辅料和原料药）与非药用级（化学试剂和食品添加剂）苯甲酸钠含量的方法。方法：采用高效液相色谱法测定含量，并采用SPSS 18.0软件对含量测定结果进行统计和比较。色谱柱为Purospher STAR LP RP-18 endcapped，流动相为乙腈-0.02％甲酸（用氨水调pH至4.0）（30∶70，V/V），流速为1.0 ml/min，检测波长为230 nm，柱温为35℃，进样量为20μl。结果：苯甲酸钠检测质量浓度线性范围为10.5～525.3μg/ml（r＝0.9999）；精密度、稳定性、重复性、耐用性试验的RSD＜0.5％；加样回收率为99.38％～101.26％（RSD＝0.56％，n＝9）。药用级与非药用级样品含量均值在99.400％～99.875％之间，非药用级样品含量均值低于药用级。结论：该方法准确、简便、专属性强、重复性好，可用于药用级与非药用级苯甲酸钠的含量测定和比较。