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HPLC-CAD法测定3种药用石斛中3种糖类成分的含量
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| 篇名： | HPLC-CAD法测定3种药用石斛中3种糖类成分的含量 |
| TITLE： | Content Determination of 3 Saccharides in 3 Kinds of Medicinal Dendrobii Caulis by HPLC-CAD |
| 摘要： | 目的：建立测定3种药用石斛中3种单/双糖成分含量的方法。方法：采用高效液相色谱-电喷雾式检测器法。色谱柱为ShodexAsahipakNH2P-504E，流动相为乙腈-水（75∶25，V/V），流速为1.0mL/min，柱温为30℃，进样量为10µL，数据采集频率为5Hz，过滤常数为5s，雾化器温度为35℃，气源为氮气，压力为4.012×105Pa。结果：果糖、D-无水葡萄糖、蔗糖检测质量浓度的线性范围分别为0.1562～1.8738mg/mL（r＝0.9995）、0.0127～0.1524mg/mL（r＝0.9997）、0.2776～3.3312mg/mL（r＝0.9998）；定量限分别为0.00261、0.00424、0.00512mg/mL，检测限分别为0.00078、0.00127、0.00154mg/mL；精密度、稳定性、重复性、耐用性试验的RSD均小于3％，加样回收率分别95.98％～98.15％（RSD＝0.83％，n＝6）、95.64％～98.62％（RSD＝1.10％，n＝6）、97.53％～98.94％（RSD＝0.53％，n＝6）；含量分别为0.28％～1.12％、0.02％～0.13％、0.76％～2.67％；总含量为1.38％～3.10％。3种石斛中糖类成分含量高低依次为蔗糖＞果糖＞D-无水葡萄糖，其中蔗糖含量及总含量高低依次均为霍山石斛＞铜皮石斛＞铁皮石斛，D-无水葡萄糖含量高低依次为霍山石斛＞铁皮石斛＞铜皮石斛，果糖含量高低依次为铜皮石斛＞铁皮石斛＞霍山石斛。结论：所建方法灵敏度高、重复性好、操作简单，可用于测定3种药用石斛中3种糖类成分的含量；3种药用石斛中糖类成分的含量存在差异。 |
| ABSTRACT： | OBJECTIVE：To establish the content determination me thod of 3 mono/disaccharides in 3 kinds of medicinal Dendrobii Caulis. METHODS ：HPLC-CAD method was established. The determination was performed on Shodex Asahipak NH2P-50 4E column with mobile phase consisted of acetonitrile-water （75 ∶ 25，V/V）at the flow rate of 1.0 mL/min. The column temperature was set at 30 ℃，and sample size was 10 µL. CAD detection condition included that data acquisition frequency was 5 Hz，filter constant was 5 s，atomization temperature was 35 ℃ ，gas source was nitrogen with pressure of 4.012 × 105 Pa. RESULTS：The linear range of fructose ，D-anhydrous glucose and sucrose were 0.156 2-1.873 8 mg/mL（r＝0.999 5），0.012 7- 0.152 4 mg/mL（r＝0.999 7），0.277 6-3.331 2 mg/mL（r＝0.999 8），respectively. The limits of quantification were 0.002 61，0.004 24 and 0.005 12 mg/mL，and the limits of detection were 0.000 78，0.001 27 and 0.001 54 mg/mL，respectively. RSDs of precision ， stability，reproducibility and durability tests were all lower than 3％. The recoveries were 95.98％-98.15％（RSD＝0.83％，n＝6）， 95.64％-98.62％（RSD＝1.10％，n＝6）and 97.53％-98.94％（RSD＝0.53％，n＝6）. The contents of them were 0.28％-1.12％， 0.02％-0.13％，0.76％-2.67％，respectively. The total content was 1.38％～3.10％. The order of saccharide content in 3 kinds of Dendrobii Caulis was sucrose ＞fructose＞D-anhydrous glucose ；the order of sucrose content and total content were Dendrobium huoshanense＞D. moniliforme ＞D. officinale ；the order of D-anhydrous glucose content was D. huoshanense ＞D. officinale ＞D. moniliforme； the order of fructose content was D. moniliforme ＞D. officinale ＞D. huoshanense . CONCLUSIONS ：Established method is sensitive ，reproducible and simple in operation ，and can be used for content determination of 3 saccharides in 3 kinds of medicinal Dendrobii Caulis. There are differences in the contents of saccharide s among 3 kinds of Dendrobii Caulis. |
| 期刊： | 2020年第31卷第10期 |
| 作者： | 郑晓倩，金传山，张亚中，刘军玲，俞年军，欧金梅 |
| AUTHORS： | ZHENG Xiaoqian，JIN Chuanshan，ZHANG Yazhong，LIU Junling，YU Nianjun，OU Jinmei |
| 关键字： | 高效液相色谱-电喷雾式检测器法；霍山石斛；铁皮石斛；铜皮石斛；单糖成分；双糖成分；含量测定 |
| KEYWORDS： | HPLC-CAD；Dendrobium huoshanense ；Den- |
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