毛细管气相色谱法测定樟脑薄荷柳酯乳膏中樟脑、薄荷脑和水杨酸甲酯

建立毛细管气相色谱法对樟脑薄荷柳酯乳膏中樟脑、薄荷脑和水杨酸甲酯含量的测定方法.使用Rtx-WAX毛细管柱,以萘为内标物,3种组分和内标在5min之内实现基线分离.各组分浓度与各峰和内标峰面积之比呈良好的线性关系,线性相关系数均大于0.999,3种组分的回收率为92.0%～102.5%.相对标准偏差小于2.0%(n=5).     

高效毛细管电泳法测定银翘解毒片中的氯原酸、甘草酸和甘草次酸

建立了同时测定银翘解每片中氯原酸、甘草酸和甘草次酸的高效毛细管电泳法,电解缓冲液为20mmol／L磷酸二氢钠和5mmol／L硼砂的混合溶液（pH7.0）。方法简便快速,具有良好的精密度、回收率和线性关系,并测定了很翘解毒片中3组分的含量。     

高效液相色谱法同时测定甘草酸及其发酵产物

建立甘草酸发酵液中甘草酸及其发酵产物乌拉尔甘草皂苷乙、3-O-β-D-葡萄糖醛酸-24-OH-18β-甘草次酸、单葡萄糖醛酸甘草次酸、18α-单葡萄糖醛酸甘草次酸和甘草次酸的RP-HPLC含量测定方法,为单葡萄糖醛酸甘草次酸的生产工艺研究及产品质量控制提供方法学基础。采用Kromasil C18(250 mm×4.6 mm,5μm)色谱柱,以甲醇(B)-1%乙酸溶液(A)为流动相进行梯度洗脱:0 min,63%B;40 min,66%B;50 min,75%B;70 min,90%B;80 min,90%B。体积流速:1.0 mL/min;进样量:10μL;柱温:25℃;检测波长:254 nm。甘草酸、乌拉尔甘草皂苷乙、3-O-β-D-葡萄糖醛酸-24-OH-18β-甘草次酸、单葡萄糖醛酸甘草次酸、18α-单葡萄糖醛酸甘草次酸和甘草次酸的线性范围分别为11.25~180.0μg/mL(r=0.9986);3.031~96.99μg/mL(r=0.9978);2.595~83.00μg/mL(r=0.9999);62.50~2000μg/mL(r=0.9999);11.25~180.0μg/mL(r=0.9980);1.560~50.00μg/mL(r=0.9992);平均回收率(n=9)分别为98.3%,101.2%,98.4%,101.9%,101.7%,97.42%,RSD分别为2.5%,1.4%,0.96%,2.8%,0.73%,0.32%。     

离子液体[BMIM]BF_4对甘草酸及其衍生物色谱行为的影响

将离子液体1-丁基-3-甲基咪唑四氟硼酸盐([BMIM]BF4)加入到高效液相色谱流动相中,研究其对甘草酸(GL)及其衍生物甘草次酸(GA)和单葡萄糖醛酸基甘草次酸(GAMG)色谱行为的影响。结果显示,加入离子液体后的流动相能够明显改善色谱峰形、减少峰拖尾、增大峰面积和峰高、提高检测灵敏度,并缩短GL,GA及GAMG 3种化合物的同时检测时间,提高检测效率。优化色谱条件为:InertSustain C18(4.6 mm×250 mm i.d.,5μm)反相色谱柱为分离柱,柱温40℃;甲醇-1.0 mmol/L[BMIM]BF4(体积比81∶19,乙酸调至pH 3.0)为流动相,流速0.7 mL/min,进样体积20μL,检测波长251 nm。GL,GA及GAMG在5.00~100 mg/L范围内线性关系良好(r≥0.999 8),检出限分别为0.02,0.04,0.09 mg/L;加标回收率分别为100.1%,98.0%,98.2%,RSD为0.18%~0.43%。同时测定GL生物转化体系中3种组分,结果满意。     

甘草次酸的电化学研究

用单扫示波极谱法研究了甘草次酸在NaAc-HAc缓冲液中（pH4．0－5．5）的电化学行为和反应机理。甘草次酸于－1．53V（vs.SCE)(P1)左右有一个二阶示波导数峰（pH＝4．0－4．9）,峰高与甘草次酸浓度在0．4－6．3μg/mL范围内呈正比,检出限为0．2μg/mL;pH在5．00－5．53之间,甘草次酸有两个还原峰,其电位分别为－1．51V（P2）和－1．57V（P3)。实验证明甘草次酸的电极过程为不可逆的逐级电子转移过程,H2O2和羟基自由基可催化甘草次酸的还原峰。     

高效液相色谱法分析测定甘草、甘草酸制品及中成药中β－型甘草次酸的含量

 报道了应用高效液相色谱法，ＳＰＣ＿（１８）色谱柱，甲醇－水－冰醋酸（７９：２０：１，Ｖ／Ｖ）流动相，ＵＶ２５４ｎｍ，以标准甘草次酸为外标，测定了甘草、甘草酸制品及中成药中甘草次酸的含量。本法适用于测定不同中成药及甘草酸制品中的甘草次酸的含量，方法简便，快速准确。     

高效液相色谱法分析测定甘草、甘草酸制品及中成药中β－型甘草次酸的含量

报道了应用高效液相色谱法，ＳＰＣ＿（１８）色谱柱，甲醇－水－冰醋酸（７９：２０：１，Ｖ／Ｖ）流动相，ＵＶ２５４ｎｍ，以标准甘草次酸为外标，测定了甘草、甘草酸制品及中成药中甘草次酸的含量。本法适用于测定不同中成药及甘草酸制品中的甘草次酸的含量，方法简便，快速准确。     

毛细管电泳叠加对比法测定阿片粉中吗啡的含量

 用毛细管区带电泳 ,以叠加对比法对阿片粉中的吗啡进行了定量分析 ,样品的回收率为 10 0 .6 % ,峰迁移时间的相对标准偏差 (RSD)不大于 2 .4 % ,相对迁移时间的RSD不大于 1.1% ,相对峰面积的RSD不大于 0 .5 1%。与内标对比工作曲线法作了比较 ,实验表明两种分析方法的结果无显著性差异 ,叠加对比法具有简便、快速、准确的优点 ,可用于样品中有效成分的快速定量。     

LC-MS/MS测定小鼠肾脏中甘草次酸的含量

建立LC-MS/MS测定小鼠肾脏中甘草次酸含量的方法.本法以原儿茶酸为内标物质,采用多反应监测模式,对肾脏中甘草次酸进行定量研究.结果所建方法灵敏、精确、快速、线性范围宽,可用于甘草次酸与雄黄联合用药小鼠肾脏中甘草次酸的含量测定.     

核磁共振定量法测定制剂中埃索美拉唑含量

以马来酸为内标,氘代二甲基亚砜为溶剂测定1H核磁共振谱,通过比较样品定量峰与内标物质响应峰峰面积,计算埃索美拉唑的含量。结果显示,同一样品在相同条件下测定6次,定量峰与内标响应峰比值的RSD为0.54%;平行配制5份样品溶液,定量峰与内标响应峰比值的RSD为0.62%。采用不同样品定量峰计算的埃索美拉唑含量分别97.2%、97.1%、98.2%、98.1%,RSD分别为0.54%、0.62%、1.33%、1.28%。本文建立的核磁共振定量法(q NMR法)可以有效避免辅料依地酸二钠、氢氧化钠干扰,经方法验证可用于测定埃索美拉唑含量。     

Preparation of Anti-Glycyrrhetinic Acid Monoclonal Antibody for Application in an Indirect Competitive Enzyme-Linked Immunosorbent Assay

Glycyrrhetinic acid is a major metabolite of glycyrrhizin, which is one of the main components of licorice roots and is considered to be one of the pharmacologically active substances in licorice. A new hybridoma cell line, named G-2A6, was generated by fusing mouse myeloma cells and splenocytes, which were immunized using glycyrrhetinic-acid–keyhole limpet hemocyanin to produce a monoclonal antibody (mAb) against glycyrrhetinic acid. Using the anti-glycyrrhetinic acid mAb, we attempted to develop a simple, rapid, and highly sensitive indirect competitive enzyme-linked immunosorbent assay (icELISA). The developed icELISA had a range from 3.91 to 125?ng/mL with low coefficients of variation (less than 5%) and demonstrated a high recovery rate of glycyrrhetinic acid spiked into licorice powder (average?=?101.76%). In addition, the icELISA could determine the glycyrrhetinic acid concentration in glycyrrhetinic-acid-spiked human serum with simple pretreatment, which suggests that the developed ELISA system using anti-glycyrrhetinic acid mAb would prove to be an effective and useful tool for determining glycyrrhetinic acid in various fields such as the analysis of Glycyrrhiza plants and pharmacokinetic studies of glycyrrhetinic acid during the administration of glycyrrhetinic acid, glycyrrhizin, and/or licorice-based medical agents.     

新型甘草次酸异噁唑衍生物的合成

以甘草次酸(脱氧甘草次酸)和3-取代苯基-5-氨甲基-异噁唑为原料, 合成了4种甘草次酸异噁唑衍生物, 通过IR, 1H NMR, 13C NMR及FABMS等方法确定了化合物的结构. 同时用L9(34) 正交试验对酰胺化反应的条件进行优化, 确定了酰化反应的最佳条件.     

电堆集富集非水毛细管电泳同时测定水杨酸、肉桂酸、阿魏酸和香草酸

建立了同时分离测定水杨酸、肉桂酸、阿魏酸和香草酸的电堆集富集-非水毛细管电泳(NACE)的新方法。运行缓冲溶液为40mmol/L乙酸钠-2.5mmol/L氢氧化钠甲醇溶液,电压-25kV,在225nm波长下紫外检测。对电压、乙酸钠浓度、氢氧化钠浓度、进样时间、样品溶液等因素对电堆集及分离的影响做了系统的研究。水杨酸、肉桂酸、阿魏酸和香草酸分别在1.4~28mg/L、0.40~8.0mg/L、0.7~18mg/L和0.7~30mg/L范围内线性关系良好(r=0.9999、r=0.9997、r=0.9994、r=0.9997);回收率分别为95.8~99.6%、96.2~98·2%、95.7~105%和98.9~103%,基于3倍信噪比(S/N=3),4种有机酸的检出限分别为0.069、0.051、0.107和0.089mg/L。     

HPTLC Densitometric Quantification of Glycyrrhizin, Glycyrrhetinic Acid, Apigenin, Kaempferol and Quercetin from Glycyrrhiza glabra

Glycyrrhiza glabra Linn., commonly known as liquorice, is a reputed drug of Ayurveda. In the present work we developed and validated densitometric methods for quantification of glycyrrhizin, glycyrrhetinic acid, apigenin, kaempferol and quercetin using HPTLC. The developed methods were found to be precise and accurate. The amount of glycyrrhizin, glycyrrhetinic acid, and quercetin was found to be 1.070, 0.84 and 0.271% w/w, respectively. Apigenin and kaempferol were quantified in free (0.007 and 0.033% w/w) as well as bound (0.021 and 0.074% w/w) forms. This is the first report of simultaneous quantification of glycyrrhetinic acid and apigenin as well as kaempferol and quercetin from G. glabra. Furthermore, no TLC densitometric methods have been reported for the quantification of apigenin, kaempferol and quercetin from G. glabra.     

HPTLC Densitometric Quantification of Glycyrrhizin,Glycyrrhetinic Acid,Apigenin, Kaempferol and Quercetin from Glycyrrhiza glabra

Glycyrrhiza glabra Linn., commonly known as liquorice, is a reputed drug of Ayurveda. In the present work we developed and validated densitometric methods for quantification of glycyrrhizin, glycyrrhetinic acid, apigenin, kaempferol and quercetin using HPTLC. The developed methods were found to be precise and accurate. The amount of glycyrrhizin, glycyrrhetinic acid, and quercetin was found to be 1.070, 0.84 and 0.271% w/w, respectively. Apigenin and kaempferol were quantified in free (0.007 and 0.033% w/w) as well as bound (0.021 and 0.074% w/w) forms. This is the first report of simultaneous quantification of glycyrrhetinic acid and apigenin as well as kaempferol and quercetin from G. glabra. Furthermore, no TLC densitometric methods have been reported for the quantification of apigenin, kaempferol and quercetin from G. glabra.

     

天然五环三萜有机功能分子

天然五环三萜在自然界中广泛存在,由六个异戊二烯单元组成,可以从动植物中分离获取。因具有手性刚性骨架、多反应位点、独特组装性能、良好生物相容性及药理活性,其在超分子化学、智能材料、界面化学、药物传输等领域有着不可忽视的潜力。本文基于课题组近年来在天然五环三萜有机功能分子方面的工作,概述了含甘草次酸和甘草酸骨架的功能小分子和高分子的设计、合成及其在水凝胶、有机凝胶、有机-无机复合凝胶、手性材料、温敏和自愈合材料、农用Pickering乳液、准聚轮烷等方面的应用。     

超临界流体萃取在甘草酸分析中的应用

对超临界流体萃取的影响因素进行了研究，并将其用于甘草酸的分析，找到了适宜的萃取条件，并与溶剂萃取方法进行了比较。     

A green and efficient protocol for large‐scale production of glycyrrhizic acid from licorice roots by combination of polyamide and macroporous resin adsorbent chromatography

A green and efficient method for large‐scale preparation of glycyrrhizic acid from licorice roots was developed by combination of polyamide and macroporous resin. The entire preparation procedure consisted of two simple separation steps. The first step is to use polyamide resin to remove licorice flavoniods from the licorice crude extract. Subsequently, various macroporous resins were tried to purify glycyrrhizic acid, and HPD‐400 showed the most suitable adsorption and desorption properties. Under the optimized conditions, a large‐scale preparation of glycyrrhizic acid from licorice roots was carried out. A 20 kg raw material produced 0.43 kg of glycyrrhizic acid using green aqueous ethanol as the solvent. The purity of glycyrrhizic acid was increased from 11.40 to 88.95% with a recovery of 76.53%. The proposed method may be also extended to produce large‐scale other triterpenoid saponins from herbal materials.     

热敏性印迹水凝胶的合成及对甘草酸分离性能的研究

以甘草酸分子为印迹分子,N-异丙基丙烯酰胺作为温度响应性单体,和甲基丙烯酸共同为甘草酸的吸附性单体,在大量交联剂存在下,N-甲基吡咯烷酮中经自由基模板聚合,制备了一种热敏性印迹凝胶,对水凝胶的热收缩动力学进行了表征;用红外光谱证实了甘草酸分子与单体分子间的相互作用,以旁证其模板作用的存在：同时还与没有模板作用所合成的同种凝胶作了实施对比,发现模板聚合所得的水凝胶可以富集水溶液中的甘草酸,并对它表现出特殊的选择性分离作用,分配系数约为非模板聚合水凝胶的11倍。