采用加压液体萃取和短端进样胶束电动色谱法同时测定何首乌水提取物中的七种亲水性生物活性化合物。
Simultaneous determination of seven hydrophilic bioactive compounds in water extract of Polygonum multiflorum using pressurized liquid extraction and short-end injection micellar electrokinetic chromatography.
作者信息
Lao Ka-Meng, Han Dong-Qi, Chen Xiao-Jia, Zhao Jing, Wang Tie-Jie, Li Shao-Ping
机构信息
State Key Laboratory of Quality Research in Chinese Medicine, Institute of Chinese Medical Sciences, University of Macau, Macao, China.
出版信息
Chem Cent J. 2013 Mar 4;7(1):45. doi: 10.1186/1752-153X-7-45.
BACKGROUND
Polygoni Multiflori Radix, He-Shou-Wu in Chinese, is a widely used traditional Chinese medicine. Clinically, water decoction is the major application form of He-Shou-Wu. Therefore, simultaneous determination of bioactive compounds in water extract is very important for its quality control.
RESULTS
A pressurized liquid extraction and short-end injection micellar electrokinetic chromatography (MEKC) were first developed for simultaneous determination of seven hydrophilic bioactive compounds in water extract of He-Shou-Wu. The influence of parameters, such as pH, concentration of phosphate, SDS and HP-β-CD, capillary temperature and applied voltage, on the analysis were carefully investigated. Optimum separation was obtained within 14 min by using 50 mM phosphate buffer containing 90 mM SDS and 2% (m/v) HP-β-CD (pH 2.5) at 15 kV and 20°C. All calibration curves showed good linearity (R2>0.9978) within test ranges. The overall LOD and LOQ were lower than 2.0 μg/mL and 5.5 μg/mL, respectively. The RSDs for intra- and inter-day of seven analytes were less than 3.2% and 4.6%, and the recoveries were 97.0%-104.2%.
CONCLUSION
The validated method was successfully applied to the analysis of He-Shou-Wu samples, which is helpful for its quality control.
背景
何首乌是一种广泛应用的传统中药。临床上，水煎剂是何首乌的主要应用剂型。因此，同时测定水提取物中的生物活性成分对其质量控制非常重要。
结果
首次建立了加压液体萃取-短端进样胶束电动毛细管色谱法（MEKC），用于同时测定何首乌水提取物中的七种亲水性生物活性成分。仔细研究了pH、磷酸盐浓度、十二烷基硫酸钠（SDS）和羟丙基-β-环糊精（HP-β-CD）浓度、毛细管温度和施加电压等参数对分析的影响。在15 kV和20℃条件下，使用含90 mM SDS和2%（m/v）HP-β-CD（pH 2.5）的50 mM磷酸盐缓冲液，14分钟内实现了最佳分离。所有校准曲线在测试范围内均显示出良好的线性（R2>0.9978）。总体检测限（LOD）和定量限（LOQ）分别低于2.0 μg/mL和5.5 μg/mL。七种分析物日内和日间的相对标准偏差（RSD）均小于3.2%和4.6%，回收率为97.0%-104.2%。
结论
该验证方法成功应用于何首乌样品的分析，有助于其质量控制。
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