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。 |
关键词: 铁皮石斛 UPLC-Q-TOF-MS 含量测定 质量控制 |
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基金项目:浙江省中医药科技计划 |
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Simultaneous Determination of Two Specific Flavonoids Glycosides in Dendrobium Officinale by UPLC-Q-TOF-MS |
luolei
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Zhejiang Institute for Food and Drug Control
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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. |
Key words: Dendrobium officinale UPLC-Q-TOF-MS content determination quality control |