摘要
目的:建立气相毛细管色谱法测定环孢素口服溶液中的乙醇和丙二醇含量。方法:色谱柱为TG-624(30 m×0.25 mm×1.4μm),采用程序升温;进样口温度:200℃;检测器温度:220℃;柱流量:0.2 mL·min^-1;进样量:1μL;进样方式:分流;分流比:20∶1;载气:氮气;内标物为正丙醇,溶剂为二甲基亚砜。结果:乙醇在1.491~3.479 mg·mL^-1的范围内,其峰面积与浓度呈良好线性关系,Y=0.5376X-0.0422,r=0.9999;高、中、低三个浓度的加样回收率分别为99.6%、100.8%、99.5%;定量限为19.9 mg·mL^-1,检测限为6.0 mg·mL^-1;重复性和中间精密度的RSD分别为0.04%﹑0.33%。丙二醇在1.4639~3.4157 mg·mL^-1的范围内线性关系良好,Y=0.3924X-0.0152,r=0.9997;高、中、低三个浓度的加样回收率分别为101.3%、100.5%、100.6%;定量限为19.5 mg·mL^-1,检测限为5.8 mg·mL^-1;重复性和中间精密度的RSD分别为0.60%﹑0.74%。批号19180021的环孢素口服溶液中乙醇和丙二醇含量分别为13.7%,12.4%;批号01916004的环孢素口服溶液中二者含量分别为13.5%,12.3%。结论:经验证,该方法简便易行,线性、专属性、耐用性、精密度、稳定性良好,可用于测定环孢素口服溶液中乙醇和丙二醇含量。
Objective:To establish a method for the determination of ethanol and propylene glycol in cyclosporine oral solution by gas chromatography(GC)with capillary colum.Methods:The column was TG-624(30 m×0.25 mm×1.4μm)using programmed temperature rise method;inlet temperature:200℃;detector temperature:220℃;column flow:0.2 mL·min^-1;injection volume:1μL;injection method:split;split ratio:20∶1;carrier gas:nitrogen;internal standard was n-propanol and solvent was dimethyl sulfoxide.Results:The peak area and concentration of ethanol in the range of 1.491 mg·mL^-1 to 3.479 mg·mL^-1 showed a good linear relationship,Y=0.5376X-0.0422,r=0.9999;the recovery rates of high,medium and low concentrations were 99.6%,100.8%,and 99.5%,respectively;LOQ was 19.9 mg·mL^-1 and LOD was 6.0 mg·mL^-1;RSD of repeatability and intermediate precision were respectively 0.04%and 0.33%.Propylene glycol show a good linear relationship in the range of 1.4639-3.4157 mg·mL^-1,Y=0.3924X-0.0152,r=0.9997;the recovery rates of high,medium and low concentrations were 101.3%,100.5%,100.6%,respectively;LOQ was 19.5 mg·mL^-1 and LOD was 5.8 mg·mL^-1;RSD of repeatability and intermediate precision were respectively 0.60%and 0.74%.The content of ethanol and propylene glycol in cyclosporin oral solution of batch number 19180021 was 13.7%,12.4%;and in batch number 01916004 was 13.5%and 12.3%,respectively.Conclusion:The validation shows that this method is simple and feasible with good linearity,specificity,durability,precision and stability.It can be used to determine the content of ethanol and propylene glycol in cyclosporine oral solution.
作者
付霞
白青山
田朋鑫
FU Xia;BAI Qingshan;TIAN Pengxin(Linyi Inspection and Testing Center,Linyi 276000,China)
出处
《中国药品标准》
CAS
2019年第6期490-494,共5页
Drug Standards of China
