摘要
目的:建立1-苯基-3-甲基-5吡唑啉酮柱前衍生化高效液相色谱法检测半夏中葡甘聚糖含量的方法。方法:使用ChomCore AQ C_(18)色谱柱(250 mm×4.6 mm,5μm),流动相A为乙腈,流动相B为0.01 mol·L^(–1)乙酸铵溶液,梯度洗脱,柱温为30℃,流速为0.8 mL·min^(–1),检测波长为250 nm。采用优化后的方法检测半夏水解后的单糖组成并对13个不同产地半夏样品和3个不同炮制品中的D-甘露糖与D-葡萄糖含量进行检测。结果:确定最佳超声提取方法为超纯水30 mL、50℃超声60 min;方法学验证结果表明,D-甘露糖、D-葡萄糖在各自质量浓度范围内线性关系良好(r≥0.99),且精密度、重复性、稳定性、加样回收率均符合要求,适用于半夏中的D-甘露糖和D-葡萄糖的检测。半夏水解后的单糖主要为甘露糖和葡萄糖,且D-甘露糖与D-葡萄糖的摩尔比为(1.47±0.06)~(1.86±0.07),证明半夏中含有葡甘聚糖。13个不同产地半夏样品和3个不同炮制品中均含有葡甘聚糖,且含量上存在差异。结论:所建立的方法具有操作简便、重复性良好和准确度高的优点。半夏中含有葡甘聚糖,且其含量会受产地及炮制方法的影响。研究结果为半夏有效成分分析和质量控制提供了技术支撑。
Objective:To establish a high performance liquid chromatography(HPLC)method with a pre-column derivatization to determine glucomannan content in Pinellia ternata(Thunb)Breit.by using 1-phenyl-3-methyl-5-pyrazolinone(PMP).Method:ChomCore AQ C_(18)(250 mm×4.6 mm,5μm)column was used with mobile phase A of acetonitrile and mobile phase B of 0.01 mol·L^(–1)ammonium acetate solution,and gradient elution was performed.The column temperature was 30℃;the volume flow rate was 0.8 mL·min^(–1),and the detection wavelength was 250 nm.The optimization of ultrasonic extraction conditions was conducted.An optimized method was used to detect the monosaccharide composition of hydrolyzed P.ternata and detect the D-mannose and D-glucose content in 13 P.ternata samples from different producing areas and three different processed products.Result:The optimal conditions for ultrasonic extraction were determined as follows:30 mL ultrapure water at 50℃for 60 minutes.The results of methodological validation showed that D-mannose and D-glucose showed good linear relationships within their mass concentration ranges(r≥0.99).The method also demonstrated satisfactory repeatability,precision,stability,and recovery rates,indicating suitability for detecting D-mannose and D-glucose in P.ternata.The monosaccharides hydrolyzed from P.ternata were mannose and glucose,with a D-mannose to D-glucose molar ratio ranging from(1.47±0.06)~(1.86±0.07),demonstrating the existence of glucomannans in P.ternata.Glucomannans were detected in all 13 P.ternata samples from various producing areas and in three processed products,with significant differences in content.Conclusion:The established method has the advantages of simplicity,high repeatability,and accuracy.The results demonstrate the presence of glucomannans in P.ternata and suggest that their content is influenced by the producing area and processing method,providing technical support for the composition analysis and quality control of P.ternata.
作者
付皎
魏璐
李金鑫
徐荣
王明星
吕建梅
冯书敏
刘大会
FU Jiao;WEI Lu;LI Jinxin;XU Rong;WANG Mingxing;LYU Jianmei;FENG Shumin;LIU Dahui(Pharmacy Faculty,Hubei University of Chinese Medicine,Wuhan 430065,China;Hubei Shizhen Laboratory,Wuhan 430065,China)
出处
《中国现代中药》
2025年第7期1255-1261,共7页
Modern Chinese Medicine
基金
国家重点研发计划项目(2023YFC3503804)
财政部和农业农村部:国家中药材产业技术体系资助项目
中央本级重大增减支项目(2060302)。
