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纸质出版日期:2020,
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郑晓倩, 金传山, 张亚中, 等. HPLC-CAD法测定3种药用石斛中3种糖类成分的含量[J]. 中国药房, 2020,31(10).
ZHENG Xiaoqian, JIN Chuanshan, ZHANG Yazhong, et al. Content Determination of 3 Saccharides in 3 Kinds of Medicinal Dendrobii Caulis by HPLC-CAD[J]. China Pharmacy, 2020,31(10).
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。
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.
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
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