白蒿挥发油成分的测定及其抗氧化活性分析

采用乙醇浸提法提取生长期和花果期白蒿的挥发油,通过正交实验确定最佳提取条件为:提取3次、浸提90 min、对于生长期和花果期白蒿液料比分别为10 mL:1 g和8 mL:1 g.通过红外光谱和液相色谱-质谱联用分析了产物的主要成分,生长期白蒿挥发油的主要成分为桉树脑、樟脑、右旋龙脑、石竹烯、Cadina-1,4-diene、白菖烯、棕榈酸乙酯等;花果期白蒿挥发油的主要成分为樟脑、石竹烯、龙脑、甲酸橙花酯等.通过1,1-二苯基-2-三硝基苯肼(DPPH)自由基清除实验对产物的自由基清除活性进行了测定,生长期和花果期白蒿挥发油对0.05 mmol/L DPPH溶液的IC50值分别为0.40和1.66 mg/mL.研究结果表明,乙醇浸提的生长期和花果期白蒿的挥发油具有较好的抗氧化活性.     

Rapid identification of chemical compositions from three species of Siegesbeckiae Herba by ultra-performance liquid chromatography-electrospray ionization-quadrupole time of flight-mass spectrometry in combination with deoxyribonucleic acid barcoding

Siegesbeckiae Herba, a traditional Chinese medicine, originates from Siegesbeckia orientalis, S. glabrescens, and S. pubescens in the Pharmacopoeia of the People's Republic of China. However, accurate identification of decoction pieces from the three plants remains a challenge. In this study, 26 batches of Siegesbeckiae Herba were identified by deoxyribonucleic acid barcoding, and their chemical compositions were determined using ultra-performance liquid chromatography-electrospray ionization-quadrupole time of flight-mass spectrometry. The results showed that the internal transcribed spacer 2 and internal transcribed spacer 1–5.8 S- internal transcribed spacer 2 sequences could distinguish three species. In total, 48 compounds were identified including 12 marker compounds screened for three species using the partial least square discriminant analysis. Among these, two diterpenoids 16-O-malonylkirenol and 15-O-malonylkirenol, and a novel diterpenoid 15,16-di-O-malonylkirenol were isolated and identified. A convenient method for the identification of Siegesbeckiae Herba was established using kirenol and 16-O-acetlydarutoside as control standards by thin-layer chromatography. Unexpectedly, none of the batches of S. orientalis contained kirenol, which did not meet the quality standards of Siegesbeckiae Herba, suggesting that the rationality of kirenol as a quality marker for S. orientalis should be further investigated. The results of this study will contribute to the quality control of Siegesbeckiae Herba.     

广藿香超临界CO_2萃取产物的GC-MS分析

采用超临界CO2 流体萃取技术从广藿香中提取出挥发油 ,挥发油得率为2.97 %(w)。采用GC -MS分离鉴定其化学组成 ,以面积归一化法测定其相对含量。从广藿香叶挥发油中鉴定出24个化合物 ,其中以广藿香醇 (48.8 % )、δ_愈创木烯 (15.2 % )、α_愈创木烯(15.3 %)等为主     

Biolabel-led research pattern reveals serum profile in rats after treatment with Herba Lysimachiae: Combined analysis of metabonomics and proteomics

In traditional Chinese medicine, Herba Lysimachiae (HL) is mainly used to treat rheumatic arthralgia. Current pharmacological studies also showed that HL has therapeutic potential for synovial diseases. HL is an oral drug, whose compounds need to enter the blood circulation before reaching the injured tissue, thus potentially causing activity or toxicity to the blood system. In this study, the biolabel-led research pattern was used to analyze the serum profile after HL intervention, based on which the safety and efficacy of HL were explored. Metabonomics and proteomics were combined to analyze the biolabels responsible for the interventions of HL in serum. Bioinformatics databases were used to screen for the material basis that may interfere with biolabels. Omics analysis showed that differentially expressed proteins (19) and metabolites (5) were identified and considered as the potential biolabels, which were involved in 8 biochemical processes (platelet activation and aggregation, blood glucose release, immune and inflammatory regulation, oxidative stress, endoplasmic reticulum stress, tumor progression, blood pressure regulation, and uric acid synthesis). Thirty-one compounds may be the material basis to interfere with 11 biolabels. The present research reveals that the potential activities and toxicities of HL can be explored based on the biolabel-led research pattern.     

Simultaneous determination of three active components in rat plasma by UPLC–MS/MS: Application to pharmacokinetic study after oral administration of Herba Sarcandrae extract

A rapid, specific and sensitive ultra‐performance liquid chromatography tandem mass spectrometry (UPLC‐MS/MS) method was developed and validated for determination of isofraxidin, rosmarinic acid and kaempferol‐3‐O ‐glucuronide in rat plasma using warfarin as an internal standard (IS). Separation was conducted on a Thermo Hypersil GOLD C₁₈ column with linear gradient elution using methanol and water. Mass spectrometric detection was conducted using selected reaction monitoring (SRM) via an electrospray ionization (ESI) source. All analytes exhibited good linearity within their concentration ranges (r > 0.9990). The lower limits of quantitations of isofraxidin, rosmarinic acid, and kaempferol‐3‐O‐ glucuronide were 1.31, 0.67 and 0.92 ng/mL, respectively. Intra‐ and inter‐day precisions of these investigated components exhibited an RSD within 11.7%, and the accuracy ranged from −12.5 to 15.0% at all QC levels. The developed method was successfully applied to a pharmacokinetic study of isofraxidin, rosmarinic acid, and kaempferol‐3‐O‐ glucuronide in rats after oral administration of Herba Sarcandrae Extract.     

反相高效液相色谱法同时测定墨旱莲中的蟛蜞菊内酯和异去甲基蟛蜞菊内酯

建立了同时测定墨旱莲中香豆草醚类成分蟛蜞菊内酯和异去甲基蟛蜞菊内酯含量的高效液相色谱法。采用Kromasil C18柱(250 mm×4.6 mm, 5 μm),流动相为甲醇-0.5%醋酸水溶液(体积比为55∶45),流速为1.0 mL/min,检测波长为351 nm,柱温为30 ℃,进样量为20 μL。在上述条件下测得的异去甲基蟛蜞菊内酯和蟛蜞菊内酯的质量浓度分别在1.6~32.0 mg/L和5.6~112.0 mg/L时与色谱峰面积之间的线性关系良好,二者高、中、低浓度条件下的平均加标回收率分别为97.5%～ 98.2%和99.0%～ 100.2%。该方法简便、快速、准确,可作为墨旱莲质量控制的一个有效方法。     

Qualitative Analysis and Componential Differences of Chemical Constituents in Taxilli Herba from Different Hosts by UFLC-Triple TOF-MS/MS

Taxilli Herba (TH) is a well-known traditional Chinese medicine (TCM) with a wide range of clinical application. However, there is a lack of comprehensive research on its chemical composition in recent years. At the same time, Taxillus chinensis (DC) Danser is a semi parasitic plant with abundant hosts, and its chemical constituents varies due to hosts. In this study, the characterization of chemical constituents in TH was analyzed by ultra-fast liquid chromatography coupled with triple quadrupole-time of flight tandem mass spectrometry (UFLC-Triple TOF-MS/MS). Moreover, partial least squares discriminant analysis (PLS-DA) was applied to reveal the differential constituents in TH from different hosts based on the qualitative information of the chemical constituents. Results showed that 73 constituents in TH were identified or tentatively presumed, including flavonoids, phenolic acids and glycosides, and others; meanwhile, the fragmentation pathways of different types of compounds were preliminarily deduced by the fragmentation behavior of the major constituents. In addition, 23 differential characteristic constituents were screened based on variable importance in projection (VIP) and p-value. Among them, quercetin 3-O-β-D-glucuronide, quercitrin and hyperoside were common differential constituents. Our research will contribute to comprehensive evaluation and intrinsic quality control of TH, and provide a scientific basis for the variety identification of medicinal materials from different hosts.     

Liquid Chromatography-Mass Spectrometry Used for Separation and Identification of Flavonoid Glycosides in Herba Epimedii Extracts

Herba Epimedii is the dried above-ground part of the genus Epimedium. Several herbs belonging to the genus Epimedium have been used in many variations of preparations and formulas for treating a wide range of diseases especially reinforcing Yang and toning the kidney by Chinese physicians for centuriesl'-~:. More than 130 chem-     

Chemical Fingerprint Analysis for Quality Control of Herba Ephedrae Based on HPLC-DAD Combined with Chemometrics Methods

A method based on high performance liquid chromatography with photodiode array detector (HPLC-DAD) was developed for chemical fingerprinting analysis of Herba Ephedrae. The index of chromatographic fingerprint's information content was utilized to optimize the fingerprint detection conditions, which reduced the time of analysis and increased the veracity of analysis greatly. Then, the similarity analysis of fingerprints was used in quality consistency evaluation of Herba Ephedrae samples. Moreover, hierarchical clustering analysis (HCA) was applied to classify the samples according to their sources and varieties. In addition, the overlapped chromatographic peaks were resolved with the help of heuristic evolving latent projection (HELP) method in order to gain the better quantitative evaluation. The results indicated that the samples could be successfully grouped in accordance with their varieties and sources. Furthermore, five marker constituents were firstly screened out to be the main chemical markers, which importantly contribute to the classification of Herba Ephedrae samples. This investigation shows that the developed methodology can be generalized to the research of quality control of herbal medicines.     

微波消解-原子吸收光谱法分析并比较不同时期地锦草中的微量元素

地锦草为大戟科地锦(Euphorbia humifusa Willd.)的干燥全草,本文采用微波消解技术对采集于不同时期的地锦草进行消解,然后利用火焰原子吸收分光光度法(FAAS)测定了不同时期地锦草中8种微量元素的含量,并且对各微量元素含量在不同时期的变化进行了研究分析。实验结果表明,不同时期地锦草中的微量元素与季节有关,元素Fe在6月的地锦草中含量最高,元素K在8月的地锦草中含量最高,地锦草中Mn在9月时含量最高,元素Na在10月份含量最高,地锦草中Ca含量在11月时最高,地锦草中的Zn,Cu和Mg含量在12月时最高,微量元素Na及Ca的变化比较跳跃,而Cu和Zn含量的变化比较缓和。研究结果可为中药地锦草采集时间的选择提供科学的依据。