高效液相色谱法测定自制苯海拉明乳膏中羟苯乙酯的含量

摘要

目的：建立测定医院自制制剂苯海拉明乳膏中羟苯乙酯的含量测定方法。方法采用高效液相色谱法（HPLC）。色谱柱：Agilent Eclipse Plus-C18（4．6 mm ×250 mm，5μm）色谱柱；流动相：甲醇-0．03 mol·L －1磷酸二氢钾溶液（含0．1％三乙胺，用50％磷酸调 pH 3．0±0．03）＝60∶40；检测波长：258 nm；柱温：25℃；流速：0．9 mL·min －1；进样体积：20μL。结果羟苯乙酯测定质量浓度在0．02～0．10 g·L －1范围内与其相应峰面积积分值呈良好线性关系（r ＝0．9995）；精密度、稳定性、重复性试验相对标准偏差（RSD）分别为1．6％、1．9％、2．0％；平均绝对回收率为92．7％，RSD 为4．3％（n ＝9）；平均相对回收率为102．5％，RSD 为3．6％（n ＝9）。结论该方法专属性、重复性、准确性较好，可用于苯海拉明乳膏中羟苯乙酯的含量测定。%Objective To establish a method of quantitative determination of ethyl hydroxybenzoate in diphenhydramine cream.Meth-ods The HPLC method was adopted with the Agilent Eclipse Plus-C18 column(4.6 mm ×250 mm,5 μm)at room temperature(25℃)and methanol-0.03 mol·L -1 phosphoric acid solution(pH adjusted to 3.0 ±0.03)(60∶40)as the mobile phase at the flow rate of 0.9 mL·min -1 .The detection wavelength for ethyl hydroxybenzoate was 258 nm,and the injection volume was 20 μL.Results The good linear relationship for ethyl hydroxybenzoate was in the range of 0.02 ~0.10 g·L -1 (r =0.999 5).RSDs of ethyl hydroxybenzo-ate for precision,stability and reproducibility tests were 1.6 %,1.9% and 2.0 %,respectively.The average absolute recovery of ethyl hydroxybenzoate was 92.7%(RSD =4.3 %,n =9),while the average relative recovery was 102.5 %(RSD =3.6 %,n =9).Con-clusions This established method was specific,accurate and reproducible for the quantitative determination of ethyl hydroxybenzoate in diphenhydramine cream.