参附注射液中3种痕量成分乌头碱、次乌头碱、新乌头碱的测定(4)
(1.School of Pharmacology， Hebei Medical University， Shijiazhuang 050017， China；
2. The Fourth Clinical Medical College of Hebei Medical University， Shijiazhuang 050011， China；
3. Institute of Forensic Science of Supreme People′s Procuratorate， Beijing 100040， China；
4. Juxian County Hospital of Traditional Chinese Medicine， Rizhao 276500， China)
[Abstract]To establish a method for the content determination of indexes for measuring aconitic compounds contained in Shenfu injection， in order to provide basis for the evaluation of the curative effect of monkshood in Shenfu injection. The sample were purified and enriched with HF，LPME. ACQUITY UPLC BEH C18 column (2.1 mm×50 mm， 1.7 μm) was adopted and eluted with a gradient program， with acetonitrile，10 mmol·L-1 NH4HCO3 (pH 10) as the mobile phases. The flow rate was 0.45 mL·min-1. The content was determined with ESI and MRM. The results showed that aconitine， hypaconitine and mesaconitine showed a good linear relationship， with r>0.999， within the range of 0.1，100 ng·L-1. The recoveries were detected to be 100.1%， 97.4%， 97.5%， with RSD being 1.2%， 1.1%， 1.5%， respectively. This method was used to prove the safety of Shenfu injection， and provide scientific basis for correct evaluation of curative effect of monkshood， as well as a reliable， simple and practical means for quality control of monkshood，containing Chinese materia medica preparations.
[Key words]aconitine； hypaconitine； mesaconitine； Shenfu injection； HF，LPME； UPLC，MS/MS
doi：10.4268/cjcmm20131013, 百拇医药(张盼盼 张俊贞 王朝虹 卢永江 蒋晔)
2. The Fourth Clinical Medical College of Hebei Medical University， Shijiazhuang 050011， China；
3. Institute of Forensic Science of Supreme People′s Procuratorate， Beijing 100040， China；
4. Juxian County Hospital of Traditional Chinese Medicine， Rizhao 276500， China)
[Abstract]To establish a method for the content determination of indexes for measuring aconitic compounds contained in Shenfu injection， in order to provide basis for the evaluation of the curative effect of monkshood in Shenfu injection. The sample were purified and enriched with HF，LPME. ACQUITY UPLC BEH C18 column (2.1 mm×50 mm， 1.7 μm) was adopted and eluted with a gradient program， with acetonitrile，10 mmol·L-1 NH4HCO3 (pH 10) as the mobile phases. The flow rate was 0.45 mL·min-1. The content was determined with ESI and MRM. The results showed that aconitine， hypaconitine and mesaconitine showed a good linear relationship， with r>0.999， within the range of 0.1，100 ng·L-1. The recoveries were detected to be 100.1%， 97.4%， 97.5%， with RSD being 1.2%， 1.1%， 1.5%， respectively. This method was used to prove the safety of Shenfu injection， and provide scientific basis for correct evaluation of curative effect of monkshood， as well as a reliable， simple and practical means for quality control of monkshood，containing Chinese materia medica preparations.
[Key words]aconitine； hypaconitine； mesaconitine； Shenfu injection； HF，LPME； UPLC，MS/MS
doi：10.4268/cjcmm20131013, 百拇医药(张盼盼 张俊贞 王朝虹 卢永江 蒋晔)