UPLC-Q-TOF-MS同时测定铁皮石斛中2个专属性黄酮苷的含量

Simultaneous Determination of Two Specific Flavonoids Glycosides in Dendrobium Officinale by UPLC-Q-TOF-MS

关键词:  铁皮石斛  UPLC-Q-TOF-MS  含量测定  质量控制

Key words:  Dendrobium officinale  UPLC-Q-TOF-MS  content determination  quality control

摘要:

目的 建立液质联用(UPLC-Q-TOF-MS)同时测定铁皮石斛中apigenin-6-C-(2′′-O-β-D-glucopyranosyl)-α-L-arabinopyranoside和apigenin-8-C-(2′′-O-β-Dglucopyranosyl)-α-L-arabinopyranoside含量的方法。方法 采用Agilent ZORBAX SB C₁₈色谱柱(2.1 mm×100 mm,1.8 μm),以乙腈(A)- 0.1%甲酸水 (B)为流动相,进行梯度洗脱,柱温为30℃,流速为0.25 mL.min_-1^,进样量为2 μL。采用电喷雾双喷离子源(Dual AJS ESI),负离子模式,质量扫描范围为100 ~ 1700 Da。结果 apigenin-6-C-(2′′-O-β-D-glucopyranosyl)-α-L-arabinopyranoside和apigenin-8-C-(2′′-O-β-D-glucopyranosyl)-α-L-arabinopyranoside分别在0.00496 ~ 0.248μg.mL_-1⁽r=0.999 9),0.01079~0.5379 μg.mL_-1⁽r=0.999 9) 内呈良好线性关系,平均加样回收率(n=6)分别为98.72%,99.87%；RSD分别为1.55%,1.59%。结论 本方法简便、快速、灵敏度高、专属性好,可为铁皮石斛药材的质量控制提供参考依据。

Abstract:

OBJECTIVE To establish an UPL-Q-TOF-MS method for the simultanious determination of apigenin-6-C-(2′′-O-β-D-glucopyranosyl)-α-L-arabino pyranoside and apigenin-8-C-(2′′-O-β-D-glucopyranosyl)-α-L-arabinopyranoside in Dendrobium Officinale. MTTHODS The separation was performed on an Agilent ZORBAX SB C₁₈ column (100 mm×2.1 mm,1.8 μm) with a mobile phase consisting of acetonitrile (A) and 0.1% formic acid water solution (B) with gradient elution at a flow rate of 0.25 mL.min_-1^, the column temperature was 30 °C and the injection volume was 2 μL. The MS spectrometry detection was performed with electrospray ionization in negative mode, the scanning rang was m/z 110 ~1700. RESULTS apigenin-6-C-(2′′-O-β-D-glucopyranosyl)-α-L-arabinopyranoside and apigenin-8-C-(2′′-O-β-D-glucopyranosyl)-α-L-arabinopyranoside were showed googd linear relationships within the ranges of 0.00496 ~ 0.248μg.mL_-1⁽r=0.999 9) and 0.01079~0.5379 μg.mL_-1 (r=0.999 9). The average recoweries (n=6) were 98.72% and 99.87%, RSD were 1.55% and 1.59%, respectively. CONCLUSION This method was simple, rapid, sensitive, with good specificity, and it can provide a reference for the quality control of Dendrobium officinale Kimura et Migo.