超高效液相色谱法测定救必应末中紫丁香苷和长梗冬青苷含量
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摘要
本研究建立了一种定性定量测定救必应末中紫丁香苷和长梗冬青苷的超高效液相色谱方法。用带有二极管阵列检测器的超高效液相色谱仪(UPLC-PAD)对救必应末中紫丁香苷和长梗冬青苷进行色谱分离和快速定量测定。以ACQUITY UPLC~(TM )C18色谱柱(2.1 mm×100 mm,1.7μm)为分离柱,柱温:35℃;流动相体系:A项为乙腈,B项为水,进行梯度洗脱;流速:0.35 mL·min~(-1);进样量:2μL;检测波长为210 nm。通过光谱图、保留时间参数对紫丁香苷、长梗冬青苷进行定性定量检测。结果表明,紫丁香苷在10～200μg·mL~(-1)的范围内线性良好(R~2=0.999);长梗冬青苷在30～600μg·mL~(-1)的范围内线性良好(R~2=0.999);方法检出限为2.5μg·mL~(-1)紫丁香苷、7.5μg·mL~(-1)长梗冬青苷,方法定量限为10μg·mL~(-1)紫丁香苷、30μg·mL~(-1)长梗冬青苷,完全满足检测需求。该方法色谱分离较好,分析速度较快,前处理简单,适用于救必应末中紫丁香苷和长梗冬青苷的定性定量检测。
An ultra-high performance liquid chromatography(UPLC) method was established for the qualitative and quantitative determination of syringin and pedunculoside in Jiubiying powder. The syringin and pedunculoside were separated and determined by UPLC instrument with diode array detector(UPLC-PAD). The ACQUITY UPLCTM C18 column(2.1 mm×100 mm, 1.7 μm) was used as separation column with the column temperature as 35℃. The mobile phase system used acetonitrile as item A and water as item B, and the gradient elution was conducted. The flow rate was 0.35 mL·min~(-1), the injection volume was 2 μL, and the detection wavelength was 210 nm. The qualitative and quantitative determination of syringin and pedunculoside were carried out by means of spectrum and retention time. The results showed that the linearity of syringin was better in the range of 10～200 μg·mL~(-1)(R~2=0.999), and that of pedunculoside was better in the range of 30～600 μg·mL~(-1)(R~2=0.999). The detection limit of this method was 2.5 μg·mL~(-1) of syringin and 7.5 μg·mL~(-1) of pedunculoside, and the quantitative limit of this method was 10 μg·mL~(-1) of syringin and 30 μg·mL~(-1) of pedunculoside, so this method could meet the testing requirements. In conclusion, this method had better chromatographic separation, higher analysis speed and simple pretreatment, so it was suitable for the qualitative and quantitative determination of syringin and pedunculoside in Jiubiying powder.
An ultra-high performance liquid chromatography(UPLC) method was established for the qualitative and quantitative determination of syringin and pedunculoside in Jiubiying powder. The syringin and pedunculoside were separated and determined by UPLC instrument with diode array detector(UPLC-PAD). The ACQUITY UPLCTM C18 column(2.1 mm×100 mm, 1.7 μm) was used as separation column with the column temperature as 35℃. The mobile phase system used acetonitrile as item A and water as item B, and the gradient elution was conducted. The flow rate was 0.35 mL·min~(-1), the injection volume was 2 μL, and the detection wavelength was 210 nm. The qualitative and quantitative determination of syringin and pedunculoside were carried out by means of spectrum and retention time. The results showed that the linearity of syringin was better in the range of 10～200 μg·mL~(-1)(R~2=0.999), and that of pedunculoside was better in the range of 30～600 μg·mL~(-1)(R~2=0.999). The detection limit of this method was 2.5 μg·mL~(-1) of syringin and 7.5 μg·mL~(-1) of pedunculoside, and the quantitative limit of this method was 10 μg·mL~(-1) of syringin and 30 μg·mL~(-1) of pedunculoside, so this method could meet the testing requirements. In conclusion, this method had better chromatographic separation, higher analysis speed and simple pretreatment, so it was suitable for the qualitative and quantitative determination of syringin and pedunculoside in Jiubiying powder.
引文
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