Determination of 5 Active Chemical Constituents in Polygonatum Sibiricum Red. by High Performance Liquid Chromatography with Dual Wavelengths
摘 要
提出了高效液相色谱-双波长法同时测定不同生长期的黄精中腺苷、人参皂苷Rb1、β-谷甾醇、香草酸和甘草素等5种活性化学成分含量的方法。样品5.000 0 g经甲醇(70+30)溶液40 mL超声提取30 min,提取液以Diamonsil钻石C18色谱柱为固定相,以0.1%(体积分数)甲酸溶液和0.1%(体积分数)甲酸-乙腈溶液的混合液为流动相进行梯度洗脱,双波长检测(λ1=252 nm,λ2=280 nm)。在优化的试验条件下,5种活性化学成分的质量浓度在0.5~100 mg·L-1范围内与其峰面积呈线性关系,检出限(3S/N)为0.36~0.47 mg·kg-1。按标准加入法进行回收试验,回收率在96.0%~101%之间,其相对标准偏差(n=6)均小于3.0%。
Abstract
A method of simultaneous determination of 5 active chemical constituents (adenosine, ginsenoside Rb1, β-sitosterol, vanillic acid and liquiritigenin) in Polygonatum Sibiricum Red. at different growth stages was proposed by high performance liquid chromatography with dual wavelengths. The sample (5.000 0 g) was extracted ultrasonically for 30 min with 40 mL of methanol (70+30) solution. The extract was separated by HPLC with dual wavelengths (λ1=252 nm, λ2=280 nm) using Diamonsil C18 column as the stationary phase, and a mixture of 0.1% (φ) formic acid solution and 0.1% (φ) formic acid-acetonitrile solution in different volume ratios as the mobile phase for gradient elution. Under the optimized test conditions, linear relationships between values of peak area and mass concentration of 5 active chemical constituents were found in the range of 0.5-100 mg·L-1, with detection limits (3S/N) in the range of 0.36-0.47 mg·kg-1. Test for recovery was made by standard addition method, giving results in the range of 96.0%-101% and RSDs (n=6) all less than 3.0%.
中图分类号 O652.63 DOI 10.11973/lhjy-hx201804006
所属栏目 工作简报
基金项目 贵州省科技厅科学技术基金项目(黔科合J字LKS[2013]08号)
收稿日期 2017/3/28
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备注刘彦东,硕士,研究方向为有机分析与检测
引用该论文: LIU Yandong,HUANG Junxue,ZHANG Quan,LIANG Xi,CHEN Wensheng. Determination of 5 Active Chemical Constituents in Polygonatum Sibiricum Red. by High Performance Liquid Chromatography with Dual Wavelengths[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2018, 54(4): 398~402
刘彦东,黄俊学,张权,梁茜,陈文生. 高效液相色谱-双波长法测定黄精中5种活性化学成分的含量[J]. 理化检验-化学分册, 2018, 54(4): 398~402
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【4】庞玉新,赵致,袁媛,等.黄精的化学成分及药理作用[J].山地农业生物学报, 2003,22(6):547-550.
【5】马红霞,周运恒,焦炳华.腺嘌呤核苷受体及其生理学作用[J].医学综述, 2004,10(10):589-590.
【6】张光辉,石力夫,胡晋红.冬虫夏草化学成分和药理作用研究进展[J].中药材, 2000,23(11):722-724.
【7】刘晓晖,朱鲲鹏,许立,等.人参皂苷Rb1的研究进展[J].武警医学院学报, 2006,15(1):82-84.
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【10】LIU C, WANG Y, XIE S, et al. Liquiritigenin induces mitochondria-mediated apoptosis via cytochrome c release and caspases activation in HeLa Cells[J]. Phytotherapy Research, 2011,25(2):277-283.
【11】CARERI M, ELVIRI L, MANGIA A. Liquid chromatography-UV determination and liquid chromatography-atomosperic pressure chemical ionization mass spectrometric characterization of sitosterol and stigmasterol in soybean oil[J]. Journal of Chromatography A, 2001,935(1/2):249-257.
【12】吴敏,卢佳,孙成均,等.HPCE法同时测定保健品及中成药中的5种苷类成分[J].华西药学杂志, 2011,26(2):165-167.
【13】WANG J, LIN T, LAI J, et al. Analysis of adenosine phosphates in HepG-2 cell by a HPLC-ESI-MS system with porous graphitic carbon as stationary phase[J]. Journal of Chromatography B Analytical Technologies in the Biomedical & Life Sciences, 2009,877(22):2019-2024.
【14】李辰,闫爱国,蔡春燕,等.蛹虫草及其培养残基中腺苷和虫草素含量的快速测定[J].色谱, 2012,30(7):711-715.
【15】常亮,陈珍珍,王栋,等.HPLC和GC-MS法测定三种黄精炮制过程中5-羟甲基糠醛的含量[J].中国药师, 2015(3):387-390.
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