高效液相色谱法测定三种羧甲司坦制剂的含量

Determine the content of carbocisteine preparations by HPLC

目的:建立测定羧甲司坦片、口服溶液和颗粒剂含量测定的RP-HPLC法。方法:以0.1%三氟乙酸溶液为流动相,流速1.0 mL·min^(-1),柱温35℃,经RP-C_(18)色谱柱洗脱,240 nm波长处测定,通过外标法计算样品的含量。结果:在本文建立的实验条件下,羧甲司坦浓度(c)在0.101 8~2.035 0 mg·mL^(-1)范围与峰面积(A)呈良好的线性关系(线性方程为A=523.12c+3.222 2,r=0.999 9),羧甲司坦的定量限为1.0×10^(-5)mg。羧甲司坦片剂的重复性为0.5%,回收率为100.9%(RSD=0.5%,n=3×3);口服溶液剂的重复性为0.2%,回收率为101.4%(RSD=0.6%,n=3×3);颗粒剂的重复性为1.0%,回收率为100.2%(RSD=0.4%,n=3×3)。结论:本实验建立的HPLC法分离效果好、灵敏度高、专属性强,可用于测定不同的羧甲司坦制剂的含量。

Objective： To establish an RP-HPLC method to determine the content of carbocisteine tablets, oral solu- tions and granules. Method： The method was established by using C18 columns and determined at the wavelength of 240 nm. The mobile phase was 0. 1% trifluoroacetic acid. The flow rate was 1.0 mL ·min^-1 and the column tem- perature was 35 ℃. The content was calculated by HPLC-external standard method. Results： The carbocisteine calibration curve was linear over the concentration range of 0. 101 8 - 2. 035 0 mg ·mL^-1 （ inear regression equation is A = 32 186c ＋ 31. 703, r = 0. 999 9）. The limit of quantification of adenosine was 1.0×10^ -5 mg. The repeat- ability and recovery of carbocisteine tablets were 0. 5% and 100. 9% （ RSD = 0. 5% , n = 3 x 3 ） , oral solutions were 0. 2% and 101.4% （RSD =0. 6% , n =3 x3）, and granules were 1.0% and 100. 2% （RSD =0. 4% , n =3 x 3 ）. Conclusion： The proposed HPLC method, with the advantagement of strong specificity, high efficiency and sensitivity, had been successfully applied in determination of the content of carbocisteine preparations.