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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