盐酸氨溴索口服液中抑菌剂及矫味剂测定方法的建立及考察  

Method establishment and investigation of bacteriostat and taste corrector assay in ambroxol hydrochloride oral solution

作　　者：王小亮 张秉华 席志芳 邓玉龙 梁亚伟 WANG Xiao-liang;ZHANG Bing-hua;XI Zhi-fang;DENG Yu-long;LIANG Ya-wei(Shanxi Institute for Food and Drug Control,Xi'an 710065,China)

机构地区：[1]陕西省食品药品检验研究院,西安710065

出　　处：《药物分析杂志》2021年第12期2227-2233,共7页Chinese Journal of Pharmaceutical Analysis

基　　金：陕西省科技厅项目(2019SF-027)。

摘　　要：目的:建立盐酸氨溴索口服液中抑菌剂及矫味剂含量测定方法并考察全国范围内该品种抑菌剂和矫味剂添加情况。方法:采用资生堂MGII C_(18)(250 mm×4.6 mm,5μm)色谱柱,以0.02 mol·L^(-1)乙酸铵溶液(用冰醋酸调节pH至4.5)-甲醇为流动相,梯度洗脱,流速1.0 mL·min^(-1),柱温为30℃,DAD检测器,检测波长为254 nm和230 nm。结果:盐酸氨溴索与4种抑菌剂、3种矫味剂色谱峰均能良好分离,并质量浓度分别在0.005~0.15 mg·mL^(-1)范围内,苯甲酸钠(r=1.000)、羟苯甲酯(r=0.9990)、羟苯乙酯(r=0.9999)、羟苯丙酯(r=1.000)、AK糖(r=0.9998)、糖精钠(r=1.000)、阿司帕坦(r=1.000),线性关系良好(n=6)。防腐剂苯甲酸钠、羟苯甲酯、羟苯乙酯、羟苯丙酯及矫味剂AK糖、糖精钠、阿司帕坦的定量下限分别为4.23、0.10、0.20、0.21、2.0、4.3、20.1 ng;平均回收率(n=9)分别为101.2%、102.3%、101.0%、101.2%、100.8%、100.2%和100.7%。对全国范围内22个生产企业的样品进行测定,个别企业抑菌剂的种类和量与生产处方不一致。结论:所建立方法准确性,专属性良好,可用于盐酸氨溴索口服液中抑菌剂及矫味剂的测定。Objective:To establish a method for assay of bacteriostat and taste corrector in ambroxol hydrochloride oral solution and to investigate the addition among samples in the whole country.Methods:The HPLC determination was performed on a Shiseido MGII C_(18)(250 mm×4.6 mm,5μm)column;the mobile phase consisted of 0.02 mol·L^(-1)ammonium acetate solution(adjusted to pH 4.5 with glacial acetic acid)and methanol with a gradient elution at the flow rate of 1.0 mL·min^(-1);the column temperatures was 30℃;DAD detector was used and detection wavelength was 254 nm and 230 nm.Results:Ambroxol hydrochloride could be well separated from 4 kinds of bacteriostat and 3 kinds of taste correctors.Good linear relationships(n=6)were achieved within the mass concentration range of 0.005-0.15 mg·mL^(-1)with sodium benzoate(r=1.000),hydroxymethyl benzoate(r=0.9990),hydroxyethyl benzoate(r=0.9999),hydroxypropyl ester(r=1.000),AK sugar(r=0.9998),saccharin sodium(r=1.000)and aspartame(r=1.000),respectively.The limits of quantitation of 4 kinds of bacteriostatfor sodium benzoate,methyl hydroxybenzoate,ethyl hydroxybenzoate,propyl hydroxybenzoate and 3 kinds of flavor correctors for AK sugar,saccharin sodium and aspartame were 4.23,0.10,0.20,0.21,2.0,4.3 and 20.1 ng,respectively.The average recoveries(n=9)were 101.2%,102.3%,101.0%,101.2%,100.8%,100.2%and 100.7%,respectively.The samples for 22 manufacturers in the whole country were determined.For several companies,the type and quantity of bacteriostat were inconsistent with the production prescription.Conclusion:The method is accurate and specific,which can be used for the determination of bacteriostat and flavor correctors in ambroxol hydrochloride oral liquid.

关 键 词：盐酸氨溴索口服液 抑菌剂 矫味剂 高效液相色谱 质量控制 

分 类 号：R917[医药卫生—药物分析学]