HPLC法测定阿司匹林原料药中的残留乙酸

Determination of acetic acid residue in aspirin by HPLC

目的建立高效液相色谱法检测阿司匹林原料药中乙酸的方法。方法采用HPLC法，ZORBAXSB—C18（4．6×250mm，5μm）色谱柱，流动相（A）磷酸溶液（0．7mL磷酸于1000mL水中，用1mol·L^-1。氢氧化钠溶液调pH为3．0）-甲醇=950：50，（B）甲醇，梯度洗脱；检测波长为210nm；流速为1．2mL·min^-1。结果乙酸在5-120μg·mL^-1。的范围内具有良好的线性（r=0．99999，n=6），回收率为99．4％，精密度RSD=0．28％。结论本方法快速，简便，准确，能满足阿司匹林产品测定乙酸残留的需要。

OBJECTIVE To establish an HPLC method for determination of acetic acid in Aspirin. METHODS HPLC with ZORBAX SB-C18 column（4.6×250mm,5μm） ,the mobile phase consisted of （A） 0.07% （mL · mL^-1 ）phosphoric acid （adjusted with 1mol · L^-1 sodium hydroxide to pH3.0）- methanol= 950 ： 50, （B） methanol; The detection wavelength was 210nm;The flow rate was 1.2mL · min^-1. RESULTS A good linear relationship was 5-120μg · mL^-1 （ r =0. 99999, n =6）, The recovery rate was 99.4 %, RSD = 0.28 %. CONCLUSION The proposed method was sensitive, accurate and simple, and can be used for the determination of acetic acid residue in Aspirin.