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

作　　者：吴俊峰 张敏娟 彭双 魏文芝 WU Junfeng;ZHANG Minjuan;PENG Shuang;WEI Wenzhi(Department of Pharmacy,Department of Medicine,Qinghai University,Xining,Qinghai,8100016 P.R.China;Qinghai Provincial Key Laboratory of Modernization of Traditional Chinese and Tibetan Medicine,NMPA Key Laboratory for Quality Control of Traditional Chinese Medicine,Tibetan Medicine,Qinghai Provincial Drug Inspection and Testing Institute,Xining,Qinghai,810016 P.R.China)

机构地区：[1]青海大学医学部药学系,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

出　　处：《华西药学杂志》2024年第1期80-83,共4页West China Journal of Pharmaceutical Sciences

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=2.1391×10^(4)X+1.4348×10^(3)、Y托品酸=6.9081×10^(4)X+5.2007×10^(4)、Y杂质Ⅰ=4.8162×10^(4)X-6.6659×10^(4),5.304~10^(6).080μg·mL^(-1)消旋山莨菪碱、5.215~52.150μg·mL^(-1)托品酸、5.300~53.000μg·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。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=2.1391×10^(4)X+1.4348×10^(3),Y=6.9081×10^(4)X+5.2007×10^(4),and Y=4.8162×10^(4)X-6.6659×10^(4),respectively.The linear range of raceanisodamine,tropic acid and impurity I were 5.304^(-1)06.080μg·mL^(-1),5.215-52.150μg·mL^(-1)and 5.300-53.000μg·mL^(-1),respectively.r were 0.9998,0.9993,and 0.9993(n=6),respectively.The average recovery of tropic acid and impurityⅠwere 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 

分 类 号：R917[医药卫生—药物分析学]