摘要
目的建立液相色谱-串联质谱法同时测定复方罗布麻片Ⅰ中9种成分的方法。方法采用ACQUITY UPLC BEH C 18色谱柱,以水:甲醇(均含0.05%甲酸)50∶50进行梯度洗脱。采用多反应监测,正负离子自动切换模式,流速:0.3 mL·min^(-1),进样量2μL。结果硫酸双肼屈嗪、防己诺林碱、粉防己碱、绿原酸、盐酸异丙嗪、蒙花苷、芦丁、金丝桃苷、氢氯噻嗪的线性范围分别为1.26~17.61μg·mL^(-1)、0.139~5.55μg·mL^(-1)、0.285~8.55μg·mL^(-1)、0.161~6.45μg·mL^(-1)、1.57~21.95μg·mL^(-1)、0.183~5.50μg·mL^(-1)、0.252~7.57μg·mL^(-1)、0.135~5.40μg·mL^(-1)、1.67~23.45μg·mL^(-1)(r为0.9975~0.9998);平均加样回收率为87.1%~98.7%,RSD为2.0%~4.1%(n=6)。结论该方法可简化提取步骤,操作简单、有效,结果准确,可实现多组分同时测定。
OBJECTIVE To establish a UPLC-MS/MS method for simultaneous determination of nine constituents in Compound Kendir Leaves TabletsⅠ.MET HODS Used ACQUITY UPLCBEH C18 column with mobile phase of water a nd methanol(both contain 0.05%formic acid)(50∶50)by gradient el ution.Multiple reaction monitoring with auto switch mode of positive and negative ions was carried out at the flow rate of 0.3 mL·min^(-1),the injection volume was 2μL.RESULTS The liner ranges were 1.26-17.61μg·mL^(-1) for dihydralazine sulfate,0.139-5.55μg·mL^(-1) for fangchinoline,0.285-8.55μg·mL^(-1) for tetrandrine,0.161-23.45μg·mL^(-1) for caffe otannic acid,1.57-21.95μg·mL^(-1) for prome thazine,0.183-5.50μg·mL^(-1) for buddleoside,0.252-7.57μg·mL^(-1)for rutin,0.135-5.40μg·mL^(-1) for hyperoside,1.67-23.45μg·mL^(-1)for hydrochlorothiazide(r=0.9975-0.9998).The average sample recovery rates were 87.1%-98.7%and RSD was 2.0%-4.1%(n=6).CONCLUSION Extraction steps can be simplified and simultaneous deter mination of polycomponents should be realized by this method.Experiment operati on was simple and effective with accutate result.
作者
许琨琨
XU Kun-kun(Quzhou Institue for Food and Drug Control,Quanzhou 362000,China)
出处
《海峡药学》
2021年第5期71-74,共4页
Strait Pharmaceutical Journal