超高效液相色谱-串联质谱法同时测定海蛇药酒中11种化学成分

Simultaneous determination of 11 kinds of constituents in seasnake medicinal liquor by ultra performance liquid chromatography- tandem mass spectrometry

中文关键词:  海蛇药酒  超高效液相色谱-串联质谱法  化学成分  含量测定

英文关键词:seasnake medicinal liquor  ultra performance liquid chromatography-tandem mass spectrometry  chemical constituents  content determination

中文摘要:

      目的 建立超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)同时测定海蛇药酒中多种成分含量的分析方法。方法 采用Agilent EC-C18色谱柱(4.6 mm×50 mm, 1.8 μm), 以水(0.1%甲酸)-乙腈(0.1%甲酸)为流动相, 梯度洗脱, 流速0.2 mL/min, 进样量为10 μL, 柱温为30 ℃; 采用电喷雾离子源(electron spray ionization, ESI)进行正离子模式监测, 多反应监测模式(multiple reaction monitoring, MRM)进行定量分析。结果 1-甲基海因、紫丁香苷、绿原酸、升麻素苷、芦丁、香草酸、木犀草苷、阿魏酸、黄芩苷、槲皮素、蛇床子素分别在0.1234~6.170 (r=0.9991)、0.03340~1.670 (r=0.9996)、0.2578~12.89 (r=0.9998)、0.3220~16.10 (r=0.9992)、0.04975~2.488 (r=0.9992)、0.02592~1.296 (r=0.9991)、0.1001~5.005 (r=0.9991)、0.1054~5.270 (r=0.9994)、0.000685~0.03425 (r=0.9986)、0.00542~0.2710 (r=0.9996)和0.2822~14.11 mg/L (r=0.9993)线性关系良好, 平均回收率在97.4%~103.5%之间, 精密度为0.34%~2.02%。结论 该方法快速、专属性强、灵敏度高, 可用于海蛇药酒的质量控制。

英文摘要:

      Objective To establish a method for simultaneous determination of 11 kinds of main active components in seasnake medicinal liquor by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods UPLC-MS/MS analysis was performed on a Agilent EC-C18 (4.6 mm×50 mm, 1.8 μm) eluted with acetonitrile and ultrapure water both containing 0.1% formic acid in a gradient program. The flow rate was 0.2 mL/min, the injection volume was 10 μL at column temperature 30 ℃. The multiple-reaction monitoring (MRM) scanning mode was employed for quantification with switching electrospray ion source polarity in positive mode. Results 1-Methylhydantoin, ligustrin, chlorogenic acid, prim-O-glucosylcimifugin, rutin, vanillic acid, luteoloside, ferulic acid, baicalin, quercetin, osthole showed a good linearity in the ranges of 0.1234?6.170 (r=0.9991), 0.03340?1.670 (r=0.9996), 0.2578?12.89 (r=0.9998), 0.3220?16.10 (r=0.9992), 0.04975 ?2.488 (r=0.9992), 0.02592?1.296 (r=0.9991), 0.1001?5.005 (r=0.9991), 0.1054?5.270 (r=0.9994), 0.000685?0.03425 (r=0.9986), 0.00542?0.2710 (r=0.9996) and 0.2822?14.11 mg/L (r=0.9993). The average recoveries varied from 97.4%?103.5%. The RSD values of precision varied from 0.34%?2.02%. Conclusions The method is rapid, specific and sensitive, and can be applied in the quality control of seasnake medicinal liquor.