基于HPLC-QQQ-MS法测定分析熏硫半夏中葫芦巴碱的含量

Determination and analysis of trigonelline content in Banxia smoked with sulfur based on HPLC-QqQ-MS

目的:建立HPLC-QQQ-MS法测定分析不同梯度的熏硫(0~150.0 g·kg^(-1))对半夏生物碱中葫芦巴碱含量的影响。方法:使用50%甲醇对半夏的葫芦巴碱进行提取,采用Inertsil ODS-3 C18(4.6×250 mm,5μm)色谱柱,以甲醇、0.1%甲酸溶液为流动相,梯度洗脱,柱温为25℃,采用电喷雾离子源,在多反应监测模式下进行正离子扫描,对半夏葫芦巴碱进行定性和定量的分析。结果:葫芦巴碱成分的线性范围在0.5~10ng之间,r>0.9990,精密度RSD均小于2.5%,重复性RSD小于0.88%,平均加样回收率95.14%,随着熏硫量的增加,半夏药材的葫芦巴碱含量先升高后降低。结论:首次建立了半夏药材的葫芦巴碱的定性和含量方法,且该方法准确稳定,重复性好,耐用性强,可以用于半夏葫芦巴碱的含量检测。

Objective:To establish a HPLC-QqQ-MS method to determine and analyze the effects of different concentration of sulfur fumigation(0~150.0 g·kg^(-1))on the contents of trigonelline in Banxia.Method:50%methanol was used to extract trigonelline from Banxia.Gradient elution was carried out using Inersil ODS-3 C_(18)(4.6×250 mm,5μm)column at 25℃,with mobile phase of methanol and 0.1%formic acid solution.ESI positive ion scanning in multi-reaction monitoring mode was set for the qualitative and quantitative analysis of trigonelline in Banxia.Result:The linear range of trigonelline in Banxia was 0.5~10 ng,r>0.9990.The precision RSD was less than 2.5%,the repeatability RSD was less than 0.88%,and the average recovery rate was 95.14%.With the increase of sulfur fumigation,the trigonelline contents of Pinellia ternata increased at first and then decreased.Conclusion:The qualitative and quantitative method of trigonelline in Banxia is established for the first time.This method is accurate,stable,reproducible and durable,which can be used for the content determination of trigonelline in Banxia.