基于LC-MS树参叶指纹图谱的建立

Establishing Fingerprint of the Leaves of Dendropanax Dentiger Based on LC-MS

目的根据树参叶液相色谱-质谱联用的分析结果,建立其液相色谱指纹图谱的鉴别方法。方法采用Waters BEH C18色谱柱(2.1 mm×100 mm,1.7μm)。流动相:乙腈(A)-0.1%甲酸(B),梯度洗脱,流速0.2 mL·min^-1,柱温35℃,进样量为1μL;电喷雾电离源(ESI),负离子检测,离子源温度为150℃,脱溶剂气温度为500℃,脱溶剂气流氮气800 L·h^-1,锥孔气流氮气50 L·h^-1,碰撞气为氩气,毛细管电压为3000 V,对树参叶主要成分进行确证。采用Waters SunfireTM C18色谱柱(4.6 mm×250 mm,5μm),流动相:乙腈(A)-混合水溶液(含甲酸0.2%和四氢呋喃0.06%)(B),梯度洗脱,检测波长256 nm,柱温30℃,体积流量1.0 mL·min^-1,分析时间80 min,进样量为5μL,建立树参叶的指纹图谱鉴别方法。结果10批样品相似度为0.939~0.989,均符合要求。结论树参为常绿植物,其叶中所含化学成分和植物的生长年限、环境、采收季节密切相关,建立的指纹图谱鉴别方法简便、重复性好,可为树参叶的品质评价提供科学依据。

OBJECTIVE To establish the HPLC fingerprint of the leaves of Dendropanax dentiger based on LC-MS.METHODS The column was Waters BEH C18(2.1 mm×100 mm,1.7μm).Mobile phase consisted acetonitrile(A)-0.1%formic acid(B)with gradient elution.Column temperature was 35℃,flow rate was 0.2 mL·min^-1 and injection volume was 1 mL.Mass spectrum condition was electrospray ionization source with negative ion detection,and the source temperature was 150℃,the desolvation temperature was 500℃,the desolvation with N2 was 800 L·h^-1,the cone with N2 was 50 L·h^-1,the collision gas was Ar,the capilary was 3000 V.HPLC with Waters SunfireTM C18(4.6 mm×250 mm,5μm)column was used.Mobile phase consisted acetonitrile(A)-aqueoussolution(B)including 0.2%formic acid and 0.06%tetrahydrofuran with gradient elution.Detection wavelength was 256 nm.Column temperature was 30℃.Flow rate was 1.0 mL·min^-1 and analytic time was 80 min.Injection volume was 5μL.Used the methods established above to be the HPLC fingerprint of Dendropanax dentiger.RESULTS Under the same fingerprint chromatogram condition,the methodological results were satisfactory to 10 batches of the samples.And the similarity range was 0.939-0.989.CONCLUSION Dendropanax dentiger is an evergreen plant.The chemical constituents in its leaves are closely related to the growth years,environment and harvesting season of the plant.The established fingerprint identification method is simple and reproducible,which can provide a scientific basis for the quality evaluation of the leaves of Dendropanax dentiger.