A New Homogenizing Technology to Obtain Rosmarinic Acid from Perilla Oil Meal

Objective To optimize the extraction technology of the active component, rosmarinic acid, an ester of caffeic acid and 3,4-dihydroxyphenyllactic acid, in perilla oil meal for the first time by a new homogenizing technology called smashing tissue extraction (STE). Methods Orthogonal design was used to optimize the extraction condition. The content of rosmarinic acid was quantified from the methanol crude extract with the help of HPLC. Results The optimization of STE process to get rosmarinic acid from the perilla oil meal was the ratio of liquid to solid material at 10:1 and the power of extraction at 150 V, extracting twice (2 min for each time). Conclusion STE could be applied to extracting the active ingredients from the oil meals due to its high extraction efficiency. This new homogenizing technology has advantages on saving extraction time, raising extraction efficiency, and maintaining the temperature sensitive constituents.     

Smashing Tissue Extraction and HPLC Determination of Paclitaxel and 10-Deacetylbaccatin from Taxus x media

Objective To optimize the extraction technology of Taxus x media by using the contents of Paclitaxel and 10-deacetylbaccatin(10-DAB) ,two representative active diterpene alkaloids of taxane type from T.x media,as evaluation standard.Methods The smashing tissue extraction(STE) of Paclitaxel and 10-DAB from T.x media,was investigated by comparing with ultrasonic extraction(UE) which was one of the modern technologies of extraction.Results STE was more efficient than UE,and the contents of 10-DAB and Paclitaxel in the extracts obtained by STE were higher than those by UE.Conclusion STE is a fast,high-performance,and energy-saving technology for the extraction of diterpene alkaloids of taxane type.STE also provides a simple,component-safe,workable,and highly efficient method for the extraction of active natural product.     

Smashing Tissue Extraction and HPLC Determination of Active Saponins from Different Parts of Panax notoginseng

Objective To optimize the extraction technology used for extracting active saponins from the roots,fibrous roots,basal part of stems,root verrucae,fruits,flowers,stems,and leaves of Panax notoginseng based on the contents of ginsengsides Rg1,Rb1,and notoginsengside R1 as evaluation indexes.Methods Different parts of P.notoginseng were extracted by smashing tissue extraction(STE),ultrasound extraction,and reflux extraction.The contents of ginsengsides Rg1,Rb1,and notoginsengside R1 in 24 kinds of extracts were determined by HPLC-UV.Hypersil C18 column(200 mm × 4.6 mm,5 μm) and acetonitrile-warter(20:80 for 30 min→45:55 for 18 min→70:30 for 2 min→80:20 for 10 min→100:0) were used;UV detector was set at 203 nm;The flow rate was set at 1.0 mL/min.Results STE was the most efficient technology with the highest yield of active saponins among the three tested extraction technologies.Conclusion STE is a fast,effective,and economical method to extract the active saponins from different parts of P.notoginseng.It could significantly shorten the extraction time and simplify the determination of the pre-processing work on identifying P.notoginseng.Such quick and effective extraction provides a powerful tool for analyzing P.notoginseng in the future.     

Optimization of Smashing Tissue Extraction Technology of Schisandra chinensis Fruits by Orthogonal Test

Objective To optimize the extract technology of active lignins from the fruits of Schisandra chinensis. Methods The content of schizandrin, gomisin A, and deoxyschizandrin were selected as standards to evaluate the efficiency of smashing tissue extraction (STE). Solid-liquid ratio, extracting times, ethanol concentration, and extracting time were investigated through orthogonal test. Results The optimized conditions for STE were ten times amount of 80% EtOH, extracting for three times, and 2 min for each time. Conclusion STE could obtain relatively higher yield, simplicity of operation, and benefit for environment protection. It could be better choice for the extraction of S. chinensis.     

Gas Chromatography–Mass Spectrometry for Quantitative and Qualitative Analysis of Essential Oil from Curcuma wenyujin Rhizomes

Objectives: A rapid and sensitive gas chromatography–mass spectrometry (GC–MS) method for quantitative and qualitative analysis of essential oil from Curcuma wenyujin rhizomes was established. Methods: The essential oil of C. wenyujin rhizomes was extracted by supercritical CO2 extraction (SFE). Six main bioactive compounds (eucalyptol, β-elemene, curzerene, germacrone, curdione, and curcumol) were analyzed in selected ion monitoring mode (SIM). Results: Curzerene is not originally present in C. wenyujin rhizomes, but is a product of the transformation of furanodiene at high temperature. The six target components demonstrated good linearity (R2 > 0.9979) over a relatively wide concentration range. The interday and intraday variations had relative standard deviation values less than 5% and the average recovery ranged from 96.95% to 100.04%. The limit of quantitation ranged from 0.032 to 0.235 μg/mL. The developed method was successfully used to analyze the six compounds in 17 samples collected from different origins. Significant variation was observed for the concentrations of the six compounds. In addition, 51 constituents were identified in C. wenyujin rhizome essential oil, consisting of 87.66% of the total essential oil, including curdione, curzerene, dehydrocurdione, germacrone, 1,4-bis(2-benzimidazoyl)benzene, neocurdione, curcumenone, and β-elemene. Conclusions: The proposed method will be useful in the quality control of C. wenyujin rhizome essential oil production.     

Aqueous Two-phase Systems with Ultrasonic Extraction Used for Extracting Phenolic Compounds from Inonotus obliquus

Objective To optimize the extracting technology of assessing the maximum yield of phenolic compounds (PC) from Inonotus obliquus by single factor experiments and orthogonal array design methods through aqueous two-phase systems combined with ultrasonic extraction. Methods The range of the independent variables, namely levels of acetone and ammonium sulfate, and ultrasonic time were identified by a first set of single factor experiments. The actual values of the independent variables coded at four levels and three factors were selected based on the results of the single factor experiments. Subsequently, the levels of acetone and ammonium sulfate, and ultrasonic time were optimized using the orthogonal array method. Results The optimum conditions for the extraction of PC were found to use 7.0 mL acetone, 5.5 mg ammonium sulfate, with ultrasonic time for 5 min. Under these optimized conditions, the experimental maximum yield of PC was 37.8 mg/g, much higher than that of the traditional ultrasonic extraction (UE, 29.0 mg/g). And the PC obtained by this method had stronger anti-oxidative activities than those by traditional UE method. Conclusion These results indicate the suitability of the models developed and the success in optimizing the extraction conditions. This is an economical and efficient method for extracting polyphenols from I. obliquus.     

Optimization of Supercritical Fluid Extraction and Rapid Resolution LC-MS/ESI Identification of Chromones from Saposhnikoviae Radix through Orthogonal Array Design

Objective To establish a rapid and effective supercritical fluid extraction(SFE) and rapid resolution liquid chromatography method coupled with diode-array detector(RRLC-DAD) to quantify the chromones in a species. Methods The effects of four parameters including ethanol concentration(50%-90%), pressure(25-45 MPa), temperature(40-60 ℃), and time(30-90 min) on the chromones yields, namely prim-O-glucosylcimifugin, cimifugin, 5-O-methylvisammioside, and sec-O-glucosylhamaudol, were investigated using SFE system with orthogonal array design(OAD). Furthermore, the extracts were analyzed using rapid resolution liquid chromatography coupled with diode-array detector(RRLC-DAD) system to confirm the results. Results Under the optimized conditions, i.e., 35 MPa of pressure, 60 ℃ of temperature, 70% ethanol, and 60 min of time, the yields of prim-O-glucosylcimifugin, cimifugin, 5-O-methylvisammioside, sec-O-glucosylhamaudol, and total chromones were 3.514, 0.132, 6.242, 0.342, and 10.231 mg/g, respectively. In comparison with ultrasonic assisted extraction(UAE), SFE was able to yield a 20.7% increase in the total chromones from Saposhnikoviae Radix. Conclusion SFE is an alternative and promising method to extract chromones from this species, and the established RRLC-DAD method could serve as a rapid and effective method for the identification of chromones from Saposhnikoviae Radix.     

Simultaneous determination and assignment of 13 major flavonoids and glycyrrhizic acid in licorices by HPLC-DAD and Orbirap mass spectrometry analyses

To determine 13 flavonoids and glycyrrhizic acid in licorice(Glycyrrhiza spp.), several samples from different areas were examined by HPLC-DAD analysisT he analysis was performed on a Zorbax Extend-C18(250 mm × 4.6 mm, 5 μm) column connected with a Zorbax Extend guard column(20 mm × 4.6 mm, 5 μm). The mobile phase consisted of(A) acetonitrile and(B) 0.026% aqueous H3PO4(V/V) using a gradient elution of 20%-25% A at 0-20 min, 25%-33% A at 20-30 min, 33%-50% A at 30-55 min, 50%-60% A at 55-65 min, and 60% A between 65 min and 80 min, and peaks were detected at 280 nm. The fourteen compounds were assigned by HPLC-Orbitrap MS methods. The regression coefficient for the linear equations for the 14 compounds ranged between 0.9998 and 1. The limits of detection and quantification lay in the range of 0.032-2.461 and 0.154-8.202 μg·mL-1, respectively. The relative recovery rates for the 14 compounds were in the range of 93.90%-106.73% with RSDs being less than 5%. Coefficient variations for intra-day and inter-day precisions were in the range of 0.27%-2.38% and 0.31%-3.51%, respectively. In summary, the validated method was applied to the simultaneous determination of the 14 components in 29 different licorice samples and was proven to be suitable for quality evaluation of licorices and their active fractions.     

响应曲面法结合灰关联度分析筛选知母中α-葡萄糖苷酶抑制剂

Objective: To screen potential α-glucosidase inhibitors from Anemarrhena asphodeloides.Methods: Response surface methodology employing Box-Behnken design was used to optimize conditions for the extraction of α-glucosidase inhibitory active compounds from A. asphodeloides. The powders(20.0 g) of A. asphodeloides were extracted under the optimized conditions. The extract was applied to a D-101 macroporous resin column. It was eluted with ethanol and water to give six fractions. Compounds from the active fraction were identified by UPLC-Q-TOF-MS. The structure-activity relationship was discussed based on grey relational analysis.Results: The optimum extraction conditions were as follows: ethanol concentration, 100%; extraction temperature, 51 ℃; and solvent to solid ratio, 23 mL/g. It indicated that the active compounds were concentrated into 80% ethanol fraction. Twenty five steroid saponins from 80%ethanol fraction were identified by UPLC-Q-TOF-MS. Peaks 19 and 23 were tentatively identified as new structures. The predicted α-glucosidase inhibitory activities of the compounds were 7 2 1 22 23 3 9 21 24 4 13 8 14 16 17 25 6 19.Conclusion: The fraction eluted by 80% ethanol showed the best inhibitory activity. After analyzing the data of UPLC-Q-TOF-MS, 25 steroid saponins were tentatively identified in this fraction.     

Relationship between Free Fatty Acid Spectrum, Blood Stasis Score, and Macroangiopathy in Patients with Type 2 Diabetes

Objective:Our aim was to investigate the correlation between free fatty acid(FFA) spectrum, blood stasis(BS) score, and macroangiopathy in type 2 diabetic patients with or without BS, as well as the possible relationship between BS and lipotoxicity. Methods: A total of 50 type 2 diabetes(T2D) patients with or without BS were enrolled from June to December 2014 in Shenzhen Traditional Chinese Medicine(TCM) Hospital, with 25 patients allocated to each of two groups. Basic information, BS score, blood glucose, blood lipids, etc., were measured for each patient. In addition, we tested the levels of interleukin(IL)?6, tumor necrosis factor α(TNF?α), and IL?18 with enzyme?linked immunosorbent assay. The macroangiopathy status of patients in the two groups was examined by color ultrasound and all factors related to BS scores were analyzed. Gas chromatography?mass spectrometry was used to explore the difference in the serum FFA spectra between the two different groups. In addition, the relationship between FFA spectra, BS scores, and macroangiopathy was analyzed. Results: BS scores, total cholesterol(TC), total triglyceride(TG), low?density lipoprotein cholesterol, IL?6, TNF?α, IL?18, carotid and femoral artery plaque, carotid intima?media thickness, carotid plaque area, and femoral artery plaque area were all significantly increased in T2D patients with BS syndrome(P 0.05). A positive correlation was observed between age, duration of diabetes, carotid intima?media thickness, carotid plaque area, femoral artery plaque area, and BS score(P 0.05). A total of 21 fatty acids were found in the serum, and total FFA(TFFA), saturated fatty acid(SFA), lauric acid(C12:0), palmitic acid(16:0), stearic acid(C18:0), arachidonic acid(C20:4n6), behenic acid(C22:0), and lignoceric acid(C24:0) scores were all found to contribute to the difference between FFA spectrums of the two groups; of the fatty acids, C12:0, C16:0, C18:0, C22:0, TFFA, and SFA positively correlated with BS scores as evaluated by Pearson's or Spearman's correlation analysis(P 0.05). Only SFA entered the regression equation in the multiple linear regression analysis. C12:0, C16:0, C18:0, C20:4n6, TFFA, and SFA were positively correlated with carotid plaque area, whereas linoleic acid(C18:3n3), Cis?5, 8, 11, 14, and 17?eicosapentaenoic acids(C20:5n3) were negatively correlated(P 0.05). C16:0 was positively correlated with the femoral artery plaque area and C18:3n3, cis?4, 7, 10, 13, 16, and 19?docosahexaenoic acids(C22:6) and nervonic acid were negatively correlated(P 0.05). Conclusion: Serum FFA spectra were significantly different between T2D patients with BS and those without, and long?chain SFA made the greatest contribution. Serum FFA spectra were correlated with BS scores and diabetic macroangiopathy, which means that lipotoxicity and BS are correlated in T2D.     

维药榲桲子脂肪酸化学成分气相色谱-质谱法分析

目的 分析榲桲子中脂肪酸成分.方法 以石油醚为提取剂,采用索氏提取法提取油脂,经氢氧化钾-甲醇甲酯化处理后,以气相色谱-质谱(GC -MS)联用技术进行分析.结果 鉴定了棕榈酸、亚油酸、油酸等12种脂肪酸,其中棕榈酸为8.30％,油酸为31.65％,亚油酸为51.86％,亚麻酸为1.90％,不饱和脂肪酸达85.46％.结论 榲桲子中脂肪酸的主要组成是不饱和脂肪酸.其中,被称为人体必需脂肪酸的亚麻酸和亚油酸的相对含量丰富,具有开发价值.     

石榴种籽油提取方法的比较

目的 研究提取石榴籽油的最佳工艺.方法 采用超临界CO2流体萃取、超声波萃取、微波萃取、溶剂回流萃取四种方法提取石榴种籽中的油脂.结果 确定最佳条件为:超临界CO2流体萃取,当萃取压力30 Mpa,分离压力:10Mpa,萃取温度:50℃,分离温度:40℃,提取2h,提取率可达17%以上.结论 通过对种籽中油脂含量及脂肪...     

小茴香超临界CO2萃取产物的成分研究

 目的:对小茴香超临界CO₂萃取产物的化学成分进行研究。方法:采用超临界CO₂萃取技术从小茴香中萃取出小茴香油，再利用GC, GC-MS和脂肪酸衍生化处理等手段，对小茴香的SFE-CQ₂产物进行了成分分析。结果:鉴定了小茴香超临界CO₂萃取产物中的14种组分，占出峰总面积的98.24%;鉴定了小茴香超临界CO₂萃取产物中的8种脂肪酸组分。结论:小茴香超临界CO₂萃取产物的主要成分是茴香脑、十八碳一烯酸、十八碳二烯酸和棕榈酸等。     

Determination of oil contents and fatty acids in seeds of Torreya Arn. in China]

OBJECTIVE: To analyze the oil contents and fatty acid composition in the seeds of Torrreya in China. METHOD: The contents and composition were determined by gravimetric analysis and GC respectively. RESULT: The oil contents in the seeds were 42.67%-54.39%. Among the fatty acids, linoleic acid and oleic acid were dominant. The unsaturated fatty acids accounted for 76.1%-82.0% of the whole fatty acids, and the major saturated fatty acids were behenic acid and palmitic acid. CONCLUSION: The oil in the seeds of Torreya is of high-quality, and the higher contents of bdhenic acid are characteristic for the oil. The development and utilization values of the seed oil in Torreya are evaluated.     

紫苏子脂肪油的超临界CO2萃取及GC—MS测定

用超临界ＣＯ２流体萃取技术从紫苏子中萃取分离出脂肪油，常法甲酯化后，用ＧＣ－ＭＳ－计算机联用技术对其进行了研究，从中分离鉴定出了１２个成分，占总脂肪油的９９．９１％，其中α－亚麻酸为主要成分，占７３．４６％。棕榈油酸等８个成分系首次从该植物中分离到。药理毒理证明，该脂肪油具有很好的调血脂作用，无毒副作用。     

响应曲面法优化超临界CO_2萃取甜杏仁油的工艺研究

目的:研究超临界CO2萃取甜杏仁油的最佳工艺条件及其成分的GC-MS分析鉴定。方法:采用响应曲面法优化甜杏仁油超临界CO2萃取工艺,并采用GC-MS对萃取的甜杏仁油进行分析。结果:建立了一个能较好预测甜杏仁油萃取率的数学模型,根据该模型,确定甜杏仁油的超临界萃取最佳工艺参数为:萃取压力27 MPa,萃取温度39℃,理论最佳萃取率为44.5%,验证三批,平均萃取率为44.0%;采用GC-MS法鉴定出16种化学成分,其中不饱和脂肪酸含量为92.6%,主要成分为油酸(83.57%)、顺-6-十八碳烯酸(5.96%)、棕榈酸(5.61%)。结论:优化后的工艺可用于甜杏仁油的提取。     

当归不同栽培品种(品系)种子含油量及组分分析

目的:对当归不同栽培品种(品系)不同成熟期种子油脂肪酸成分进行定性定量分析。方法:采用索氏提取法提取样品,气相色谱-质谱(GC-MS)联用技术进行成分分析。结果:综合运用MassworksTM质谱解析软件、谱库检索等解析手段鉴定出当归种子油中11种脂肪酸成分,对样品进行主成分分析,得出己酸、油酸、癸酸是当归不同栽培品种(品系)不同成熟度种子共有的特征性脂肪酸组成;对样品进行聚类分析可将当归不同栽培品种(品系)不同成熟度种子样品进行分类。结论:确定当归主产地种子最佳采收期为8月22日至8月30日;建议岷归3号、岷归4号可以作为重点推广的优良品种。     

菜籽油脚中天然VE和脂肪油的超临界CO2萃取分离及其GC—MS分析

本文首次用超临界CO_2萃取菜籽油下脚料中的天然V_E和脂肪油,并用GC-MS联用技术对萃取物中天然V_E进行了含量测定,将萃取的脂肪油进行了GC-MS分析。结果表明,超临界CO_2萃取能从油下脚料中萃取出天然V_E,萃取物中V_E的含量比原料(油脚)提高5倍左右,V_E的萃取率达95％;所萃取的脂肪油中含有10种脂肪酸,主要成分为油酸、亚油酸及亚麻酸等,其中亚油酸和亚麻酸等人体必须脂肪酸含量明显提高,芥酸的含量大大低于食用菜籽油的水平。     

中药木鳖子中脂肪酸的气相色谱-质谱联用分析

目的：测定中药木鳖子中的脂肪酸成分。方法：以石油醚为溶剂，采用索氏提取法提取其脂肪酸。经甲酯化处理后，用GC／MS联用仪对其脂肪酸组成进行了分析和鉴定。结果：共分离出14种脂肪酸，占脂肪酸总量的89．23％。结论：木鳖子脂肪酸中不饱和脂肪酸占41．91％，且大部分是具生物活性物质。