UHPLC-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 2 Specific Flavonoids Glycosides in Dendrobium Officinale by UHPLC-QTOFMS

目的建立液质联用(UHPLC-Q-TOF-MS)同时测定铁皮石斛中apigenin-6-C-(2''-O-β-D-glucopyranosyl)-α-Larabinopyranoside和apigenin-8-C-(2''-O-β-D-glucopyranosyl)-α-L-arabinopyranoside含量的方法。方法采用Agilent ZORBAX SB C_(18)(2.1 mm×100 mm,1.8μm)色谱柱,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2μL。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m/z100~1 700。结果 Apigenin-6-C-(2''-O-β-D-glucopyranosyl)-α-L-arabinopyranoside和apigenin-8-C-(2''-O-β-D-glucopyranosyl)-α-Larabinopyranoside分别在0.004 96~0.248μg·mL^(-1)(r=0.999 9)、0.010 79~0.537 9μg·mL^(-1)(r=0.999 9)内呈良好线性关系,平均加样回收率分别为99.04%、100.41%;RSD分别为2.09%、2.00%。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。

OBJECTIVE To establish an UHPLC-Q-TOF-MS method for the simultaneous 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.METHODS The separation was performed on an Agilent ZORBAX SB C18(100 mm×2.1 mm,1.8µm)column 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℃and the injection volume was 2µL.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 good linear relationships within the ranges of 0.00496–0.248μg·mL^(-1)(r=0.9999)and 0.01079–0.5379μg·mL^(-1)(r=0.9999).The average recoveries were 99.04%and 100.41%,RSD were 2.09%and 2.00%,respectively.CONCLUSION This method is simple,rapid,sensitive,with good specificity,and it can provide a reference for the quality control of Dendrobium officinale.