手性高效液相色谱法测定板蓝根中表告依春和告依春含量

采用Chiralpak IC手性柱(250 mm×4.6 mm, 5 μm),建立了正相高效液相色谱测定板蓝根中表告依春(R-告依春)和告依春(S-告依春)含量的方法。考察了流动相组成、流速和柱温对分离度的影响。经优化后的实验条件: 以正己烷-异丙醇(体积比为90:10)为流动相,流速为0.8 mL/min;检测波长为245 nm,柱温为20 ℃。在此优化条件下,表告依春和告依春分离度为3.4,检出限为2.0 mg/L,在0.02～2.0 g/L范围内有良好的线性关系,平均回收率为101%,相对标准偏差(RSD)小于3.0%(n=6)。本方法可将具有抗病毒活性的表告依春与其对映体告依春基线分离并测定,专属性强,能有效控制板蓝根的质量。     

微波消解电感耦合等离子体发射光谱法测定葛根中钾元素的研究

本文研究了葛根样品的不同消解方法,提出了用微波消解电感耦合等离子体发射光谱法（ICP－AES）测定葛根中微量元素钾的方法。测定方法的检测限达0.0043μg/ml。方法的相对标准偏差（RSD）为0．52％。试样经过微波消解后,测定的平均回收率为103．2％,具有灵敏、准确及快速测定的特点。     

植物草乌毒蛋白的分离及性质

介绍草乌毒蛋白提取方法。草乌根经ＰＨ７．２５ ＰＢＳ溶液（含９ｇ＝／ＬＮａＣｌ）浸提,浸提液经ＣＭ－ＳＦＦ柱和ＳｅｐｈａｃｒｙｌＳ－２００凝胶过滤柱分离,然后在高效凝胶过滤柱上制德ＡＣＯ毒蛋白,利用光电二极管列检测器的光谱性能确认色谱峰的纯度,并根据标准蛋白的相对分子质量校正曲线求得ＡＣＯ的相对分子质量,用柱后衍生荧光法测定了其氨基酸组成。     

银黄口服液的质量控制及其高效液相色谱指纹图谱的研究

利用高效液相色谱方法,建立了复方银黄口服液及其原料药材黄芩和金银花的指纹图谱,测定了银黄口服液中黄芩苷 和绿原酸的含量。以Lichrospher C18色谱柱(250 mm×4.6 mm i.d.,5 μm)为分离柱,以甲醇和0.1%磷酸水溶液为流动 相进行二元梯度洗脱,流速0. 6 mL/min,在254 nm波长下检测。采用夹角余弦和相关系数的方法,计算6批银黄口服液指 纹图谱的相似度均在0.99以上,表明银黄口服液的质量未见显著差异。将银黄口服液指纹图谱中的共有峰与原料药材黄芩 和金银花的指纹图谱中的共有峰相比较,对其归属进行确认,大部分共有峰可以匹配。     

不同极性的溶剂与黄芪饮片在微波场中升温行为的研究

研究了水(强极性)、无水乙醇(中等极性)、正己烷(弱极性)分别与中药饮片组成的体系在微波作用下饮片内部以及溶剂主体温度的升温规律,发现在微波辐射下,3个体系中饮片内部的温度均大于溶剂主体温度,形成了由内到外的温度梯度,内外温度梯度的大小为正己烷-黄芪>无水乙醇-黄芪>水-黄芪。由此得出微波辐射下饮片内部与溶剂主体之间形成的温度梯度与有效成分的传质方向一致。而在常规加热情况下,温度梯度与传质方向是相反的。     

黄芩中黄芩苷的亚临界水提取及高效液相色谱分析

建立了黄芩药材中黄芩苷的亚临界水提取 高效液相色谱测定方法。分别考察了温度、压力、提取时间、提取物颗粒度、溶剂比等因素对提取量的影响,并与有机溶剂提取法比较。结果表明,当两者具有相同的提取效果时,亚临界水提取法的提取时间及提取溶剂的消耗量大大减少,避免了使用有机溶剂造成的污染。黄芩苷提取最佳条件为:样品颗粒度80～100目,溶剂比0.2 mL/mg ,5 MPa,130 ℃保持10 min。并通过提取 高效液相色谱联机分析实现了对提取物的实时监测。该技术有望成为从中药材中提取脂溶性成分的有效方法。     

Qualitative identification and quantitative comparison of Physochlainae Radix from different regions based on chemometric methods

Physochlainae Radix (PR) is an essential herbal medicine that has been generally applied for treating cough and asthma. In this study, a comprehensive strategy for quality evaluation of PR from different origins was established by integrating qualitative identification, quantitative analysis, and chemometric methods. A total of 58 chemical components were identified by ultra-high-performance liquid chromatography coupled with quadrupole time-of-flight tandem mass spectrometry (UHPLC-Q-TOF-MS/MS), and a sensitive and rapid UHPLC-QqQ-MS/MS method was established for the simultaneous determination of 12 compounds. In addition, multivariate statistical analysis was applied for discriminant analysis to compare the differences among 30 batches of PR samples. The results showed that the 30 batches of PR collected from four provinces could be clustered into three categories, in which scoparone, protocatechuic acid, tropic acid, and scopolin were important components to distinguish the primary and non-primary producing areas, as well as superior and inferior products of PR. Chemometric results were consistent and validated each other, and systematically explained the intrinsic quality characteristics of PR. This study first demonstrated that LC-MS combined with multivariate statistical analysis, provided a comprehensive and effective means for quality evaluation of PR.     

Ultrasound-assisted preparation of ‘Ready-to-use’ extracts from Radix Paeoniae Rubra with natural deep eutectic solvents and neuroprotectivity evaluation of the extracts against cerebral ischemic/ reperfusion injury

Natural deep eutectic solvent (NaDES) is widely applied in the extraction of nutrients from natural resources as a greener alternative for fossil solvent. In the present work, 27 different NaDESs were screened for the extraction of paeoniflorin (PF) and galloyl paeoniflorin (GPF) from Radix Paeoniae Rubra (RPR). After screening and extraction parameter optimization, the extraction yields of PF and GPF reached up to 182.8 mg/g and 77.4 mg/g with the selected NaDES, ChCl-Sor. Furthermore, the antioxidant activity in vitro and neuroprotectivity in vivo of the ‘ready-to-use’ extracts were evaluated comprehensively. Especially in vivo, the cerebral ischemic/ reperfusion injury model was established in rats and the protective effects of the RPR extracts were determined. The results not only proved that NaDES is a valuable green extraction media, but also indicated the safety and potential pharmaceutical application of NaDES based ‘ready-to-use’ extracts from medical plants.     

黄芩及其制剂中黄芩素和黄芩甙的

用毛细管区带电泳 -电化学检测法测定了黄芩及其制剂中黄芩素和黄芩甙的含量。研究了电极电位、电解液酸度和浓度、电泳电压及进样时间等对电泳的影响 ,得到了较为优化的测定条件。以直径为300μm的碳圆盘电极为检测电极 ,电极电位为0.90V(vsSCE) ,在100mmol/L硼酸盐缓冲液(pH9.0)中 ,上述两组分在8min内完全分离。黄芩素和黄芩甙浓度与电泳峰电流分别在5.0×10 -7～1.0×10 -3mol/L和1.0×10 -6～1.0×10 -3mol/L范围内呈良好线性 ,检出限分别为2.24×10 -7mol/L和5.48×10 -7mol/L。7次测定分别含5.0×10 -4mol/L黄芩素和黄芩甙试样溶液 ,峰高的相对标准偏差分别为3.53%和4.03%。