摘要
目的:建立肺炎合剂中盐酸麻黄碱的鉴别和含量测定方法。方法:(1)薄层鉴别:溶液取5μL,使用硅胶G薄层板,展开剂为正丁醇-冰醋酸-水(8∶2∶1),显色剂为茚三酮试液,在105℃下加热显色。(2)含量测定:色谱柱为Capcell PAK C18(150 mm×4.6 mm,5μm),流动相为乙腈:0.1%磷酸(含三乙胺0.1%)(6∶94),检测波长为210 nm,流速为0.9 m L·min^-1,柱温30℃,进样量为10μL。结果:(1)供试品色谱中,在与对照品色谱相应的位置上,显相同的红色斑点。(2)盐酸麻黄碱在0.42-2.12μg范围内,线性范围良好(r=0.9999),平均回收率为98.12%,RSD为1.10%(n=6)。结论:薄层色谱法可以用于肺炎合剂中盐酸麻黄碱的鉴别。高效液相色谱法简便、准确、灵敏度高,重复性好,可用于肺炎合剂中盐酸麻黄碱的含量测定。
Objective: To establish a method for the discrimination and content determination of Ephedrine Hydrochloride in pneumonia mixture.Methods:(1) TLC:Take the test and reference solutions of ephedrine hydrochloride both for 5μL.Point on the same silica gel G plate.N-butanol-acetic acid-water(8 ∶ 2 ∶ 1) as the agent,started out,dried,sprayed with ninhydrin test solution,heated at 105 ℃ to spot the color clear.(2) Content determination:Agilent C18(150mm × 4.6 mm,5 μm) was used as the column and acetonitrile-0.1% phosphoric acid(0.1% Triethylamine)(6 ∶ 94)was used as the mobile phase at a flow rate of 1.0 m L·min^-1and the column temperature was 30 ℃ and the detection wavelength was set at 210 nm.The quantity of injection was 10 μL.Result:(1) On the chromatography of testing products,chromatography with reference substance corresponding position had the same red spots.This method can be used in the identification of Pneumonia Mixture of ephedrine hydrochloride.(2) The calibration curve of Ephedrine Hydrochloride was linear in ranger of 0.42 - 2.12 μg(r = 0.999 9).The average recovery rate was 98.12% and RSD was 1.10%(n= 6).Conclusion: The method is simple,accurate and has high sensitivity and good repeatability on the content determination of Pneumonia Mixture of ephedrine hydrochloride.
出处
《中华中医药学刊》
CAS
北大核心
2016年第12期2993-2997,共5页
Chinese Archives of Traditional Chinese Medicine
基金
江苏高校品牌专业建设工程项目(PPZY2015A097)
江苏省高等学校大学生创新创业训练计划项目(201512682017X)
关键词
肺炎合剂
盐酸麻黄碱
薄层鉴别
HPLC
Pneumonia Mixture
Ephedrine hydrochloride
thin layer chromatography
HPLC