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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 Δ

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郑晓倩 ，金传山 ，张亚中 ，刘军玲 ，俞年军 ，欧金梅（1.安徽中医药大学药学院，合肥 230012；2.安徽省食
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品药品检验研究院，合肥 230051）
中图分类号 R282.71；R917 文献标志码 A 文章编号 1001-0408（2020）10-1185-05
DOI 10.6039/j.issn.1001-0408.2020.10.06
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
Shodex Asahipak NH2P-50 4E，流动相为乙腈-水（75 ∶ 25，V/V），流速为1.0 mL/min，柱温为30 ℃，进样量为10 µL，数据采集频率为
5
5 Hz，过滤常数为5 s，雾化器温度为35 ℃，气源为氮气，压力为4.012×10 Pa。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 0.156 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）；
定量限分别为 0.002 61、0.004 24、0.005 12 mg/mL，检测限分别为 0.000 78、0.001 27、0.001 54 mg/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。
关键词 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
Content Determination of 3 Saccharides in 3 Kinds of Medicinal Dendrobii Caulis by HPLC-CAD
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ZHENG Xiaoqian ，JIN Chuanshan ，ZHANG Yazhong ，LIU Junling ，YU Nianjun ，OU Jinmei（1. College of
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Pharmacy，Anhui University of TCM，Hefei 230012，China；2. Anhui Institute for Food and Drug Control，
Hefei 230051，China）
ABSTRACT OBJECTIVE：To establish the content determination method 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
5
Hz，filter constant was 5 s，atomization temperature was 35 ℃ ，gas source was nitrogen with pressure of 4.012 × 10 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 saccharides among 3 kinds of Dendrobii Caulis.
KEYWORDS HPLC-CAD；Dendrobium huoshanense；Den-
Δ 基金项目：国家自然科学基金资助项目（No.U19A2009）；中央 drobium officinale； Dendrobium moniliforme； Monosaccha-
财政林业科技推广示范资金项目（No.林科函〔2019〕357号）；中央财政
rides；Disaccharides；Content determination
林业改革发展资金项目（No.皖财资环〔2019〕722 号）；安徽省财政厅
“特支计划”资金项目（No.皖财行〔2019〕669号）
＊硕士研究生。研究方向：中药质量标准。E-mail：185078352@qq.
石斛属（Dendrobium）是兰科大属植物之一 ，分布
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com
# 通信作者：教授，硕士生导师。研究方向：中药炮制学教学与 极其广泛。《中国植物志》中记载的石斛药用品种有近51
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科研。E-mail：jcs4@sohu.com 种 ，其中安徽霍山境内及其邻近山区主产的霍山石斛

中国药房 2020年第31卷第10期 China Pharmacy 2020 Vol. 31 No. 10 ·1185 ·