液相色谱-串联质谱法测定复方罗布麻片Ⅰ中9种成分含量

Simultaneous Determination of Nine Constituents in Compound Kendir Leaves TabletsⅠby UPLC-MS/MS

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.