高效液相色谱-质谱-电雾式检测法同时测定辛夷提取物中4种木脂素成分

Simultaneous Determination of Four Lignans in Magnoliae Flos Extract by High Performance Liquid ChromatographyElectrospray Ionization Mass Spectrometry

建立了高效液相色谱-质谱-电雾式检测器（ HPLC-MS-CAD）联用技术同时测定辛夷中4种木脂素类成分的定量分析方法。采用 YMC-Pack ODS-A（250 mm×4.6 mm,5μm）色谱柱,甲醇-水梯度洗脱,柱温25℃,流速1 mL/min,检测波长278 nm,紫外检测器后3：7分流,分别进入质谱和电雾式检测器进行检测。以木兰脂素为内参物,建立松脂素二甲醚、里立脂素B二甲醚和表木兰脂素A与内参物的相对校正因子,并进行含量计算,实现一测多评。同时采用外标法测定辛夷提取物中4种木脂素成分的含量,比较计算值与实测值的差异,验证所建立方法的准确定。本方法对松脂素二甲醚、木兰脂素、里立脂素B二甲醚和表木兰脂素A 4种木脂素类成分的检出限分别为0.34,0.55,0.50和0.58 mg/L,线性范围分别为6.8～270 mg/L,11～546 mg/L,2.0～100 mg/L 和2.3～116 mg/L,相关系数为0.9995～0.9998,加样回收率（ n=9）为98.2％～99.5％,采用校正因子计算的含量值与外标法计算的含量值之间无显著差异,所建立的方法准确、可行,可用于中药辛夷的质量评价。

A high performance liquid chromatography-electrospray ionization mass spectrometry- charged aerosol detection （HPLC-MS-CAD） method was established for the simultaneous quantitative analysis of four Lignans in Magnoliae Flos extract. The components were separated on a YMC-Pack ODS-A column （250 mm× 4.6mm, 5 μm） by gradient elution with methanol and water as the mobile phase at aflow rate of 1.0 mL/min. Then the elution solution was routed into MS equipment at a flow rate of 0.3 mL/min and CAD detector at a flow rate of 0.7 mL/min by a split ratio of 3 ： 7 for the further detection. The column temperature was 25 ℃ and the detection wavelength was 278 nm. A method was developed for the quantitative analysis of muti-components by single maker （QAMS） to determine pinoresinol dimethylether, magnoli, l irioresinol B dimethylethe and epi- magnoli A . Magnoli was selected as internal standard and the relative correction factors （RCF） of the four Lignans were calculated. The contents of the four Lignans in Magnoliae Flos extract were determined by both external standard method and QAMS. The QAMS method was evaluated by comparison of its assay result and that of external standard method. Under the selected chromatographic condition, the limits of detection of pinoresinol dimethylether, magnoli, lirioresinol B dimethylethe and epi-magnoli A were O. 34, 0.55, 0. 50 and 0.58 mg/L, respectively, while the linear range were within 6. 8-270 mg/L, 11- 546 mg/L, 2.0-101 mg/L and2.3-116 mg/L. The recoveries （n=9） were 98.2%-99.5%, and the correlation coefficient were 0. 9995-0. 9998. No significant differences were found between the quantitative results of external standard method and QAMS method. The developed method is accurate, feasible, and can be used for quality evaluation of Magnoliae Flos .