摘要
目的建立气相色谱法(GC)测定异维A酸原料药中吡啶和乙酸的方法。方法色谱柱为DB-WAXETR毛细管柱(30 m×0.320 mm,1.00μm),进样口温度220℃,氢火焰离子化检测器温度250℃;载气为氮气,流速2.0 mL·min^(-1),分流比5∶1。直接进样,初始温度为110℃,保持12 min,以50℃·min^(-1)升温至220℃,保持5 min,进样体积为1.0μL。结果吡啶和乙酸的线性范围分别为4.74~94.8μg·mL^(-1)、25.4~508.0μg·mL^(-1),线性方程分别为Y=1.953 2X-0.722 5(r=0.999 5)、Y=2.334X-4.108 9 (r=0.999 6);平均回收率分别为89.69%、84.59%,RSD分别为5.5%、3.3%;检测限分别为1.23,0.84μg·mL^(-1),定量限分别为4.09,2.79μg·mL^(-1)。结论建立的气相色谱法适用于异维A酸原料药中吡啶和乙酸测定。
OBJECTIVE To establish a gas chromatography method for determination of pyridine and acetic acid in Isotretinoin.METHODS DB-WAXETR( 30 m× 0.320 mm,1.00 μm) capillary column was used. The injection port temperature was 220 ℃ and FID temperature was 250 ℃.Nitrogen was the carrier gas with flow rate of 2. 0 mL·min^-1 and split ratio 5 ∶ 1. Samples were tested by direct injection.The oven temperature was initially held at 110 ℃ for 12 min and then programmed to 220 ℃ at 50 ℃·min^-1 and held for5 min.The injection volumn was 1.0 μL. RESULTS The linear ranges of pyridine and acetic acid were respectively 4.74-94.8 μg·mL^-1,25.4-508.0 μg·mL^-1 and regression equations were Y = 1.953 2 X-0.722 5( r = 0.999 5),Y = 2.334 X-4.108 9( r = 0.999 6).The average recoveries were 89.69%,84.59% and RSDs were 5.5%,3.3%. LODs were 1.23,0.84 μg·mL^-1 and LOQs were 4. 09,2.79 μg·mL^-1.CONCLUSION The method can be applied in determination of pyridine and acetic acid in Isotretinoin.
作者
唐杨
TANG Yang(Chongqing Institute For Food and Drug Control,Chongqing Engineering Research Center for Pharmaceutical Process and Quality Control,Chongqing 401121,China)
出处
《今日药学》
CAS
2019年第2期83-85,89,共4页
Pharmacy Today
基金
国家药典委员会国家药品标准提高研究项目(食药监办药化管[2016]141号)