UPLC测定消旋山莨菪碱片中的有关物质
Determination of related substances of Raceanisodamine tablets by UPLC
吴俊峰 1张敏娟 2彭双 2魏文芝2
作者信息
- 1. 青海大学医学部药学系,青海西宁 810016;青海省药品检验检测院国家药品监督管理局中药(藏药)质量控制重点实验室青海省中藏药现代化研究重点实验室,青海西宁 810016
- 2. 青海省药品检验检测院国家药品监督管理局中药(藏药)质量控制重点实验室青海省中藏药现代化研究重点实验室,青海西宁 810016
- 折叠
摘要
目的 采用UPLC-PDA法测定消旋山莨菪碱片中的有关物质.方法 采用C18柱,以0.01 mol·L-1磷酸二氢钾溶液(含0.15％三乙胺溶液,磷酸调pH6.5)-甲醇(70:30)为流动相,流速0.2 mL·min-1,检测波长220 nm.结果 消旋山莨菪碱、托品酸、阿托酸6β-羟基-3α-托品酯(杂质Ⅰ)的线性回归方程分别为:Y消旋山莨菪碱=2.1391 × 104X+1.4348 × 103、Y托品酸=6.9081 × 104X+5.2007 × 104、Y杂质Ⅰ=4.8162 × 104X-6.6659 × 104,5.304～106.080 µg·mL-1消旋山莨菪碱、5.215～52.150 µg·mL-1托品酸、5.300～53.000 µg·mL-1杂质Ⅰ与峰面积呈良好的线性关系,r分别为0.9998、0.9993、0.9993(n=6).托品酸、杂质 Ⅰ 的平均回收率分别为 97.21％、100.24％,RSD分别为 1.78％、0.67％.结论 所用方法准确度高、专属性强、重复性好,可用于测定消旋山莨菪碱片中的有关物质.
Abstract
OBJECTIVE To determine the related substances of Raceanisodamine tablets by UPLC.METHODS A C18 column was used and 0.01 mol·L-1 potassium dihydrogen phosphate solution(containing 0.15％triethylamine solution,using phosphoric acid to adjust pH to 6.5)-methanol(70:30)as mobile phase,flow rate was set at 0.2 mL·min-1,and the detection wavelength was 220 nm.RESULTS The linear regression equations of raceanisodamine,tropic acid and 6β-hydroxy-3α-tropine atoate(impurity Ⅰ)were Y=2.1391 × 104X+1.4348 × 103,Y=6.9081 × 104X+5.2007 × 104,and Y=4.8162 x 104X-6.6659 x 104,respectively.The linear range of raceanisodamine,tropic acid and impurity Ⅰ were 5.304-106.080 μg·mL-1,5.215-52.150 μg·mL-1 and 5.300-53.000 μg·mL-1,respectively.r were 0.9998,0.9993,and 0.9993(n=6),respectively.The average recovery of tropic acid and impurity Ⅰ were 97.21％and 100.24％with RSD 1.78％and 0.67％.CONCLUSION This method has high accuracy,strong specificity and good repeatability,which can be used to determine the related substances and content of Raceanisodamine tablets.
关键词
超高效液相色谱法/消旋山莨菪碱片/生物碱/消旋山莨菪碱/托品酸/阿托酸6β-羟基-3α-托品酯/有关物质/解痉药物/异构体Key words
UPLC/Raceanisodamine tablets/Alkaloid/Raceanisodamine/Tropic acid/Atropic acid 6 β-hydroxyl-3 α-tropine ester/Related substances/Antispasmodic drugs/Isomers引用本文复制引用
出版年
2024
NETL
NSTL
万方数据