辐照灭菌对川芎中阿魏酸含量的影响

用高效液相色谱法对经辐照灭菌前后的川芎药材中阿魏酸的含量进行测定,比较灭菌前后阿魏酸含量变化情况。方法:采用Accurasil-C1(8250mm×4.6mm 5μm),流动相为甲醇-水-磷酸(30∶70∶0.05),检测波长320nm色谱条件进行含量测定。结果:阿魏酸在0.02268～0.11340μg范围内线性关系良好,平均回收率为101.387%,其RSD为1.52%。灭菌前后及灭菌饮片与粉末中阿魏酸含量产生显著性变化。结论:以阿魏酸为指标表明川芎药材不适宜在10K格瑞辐照剂量下进行灭菌。     

化妆品中芦荟的质量标准研究

通过薄层色谱法对化妆品中芦荟进行定性鉴别,并考察不同厂家、温度、相对湿度条件下对薄层色谱分离效果的影响,采用高效液相色谱法测定化妆品中芦荟苷含量。实验结果表明,供试品薄层色谱图斑点清晰、专属性强,与对照品、对照药材色谱图斑点均呈现良好的对应关系,可作为芦荟的定性鉴别依据;芦荟苷在0.209 0～4.180 0 μg内与峰面积呈现良好线性关系,加样回收率为101.9%～102.7%,RSD为0.31%。该法简便、稳定、可靠,可作为化妆品中芦荟的质量控制方法。     

川芎-香附药对挥发性成分谱的GC-MS分析

目的:分析川芎-香附药对挥发性成分谱的化学组成。方法:采用水蒸汽蒸馏改进法提取挥发油、GC-MS测定供试品,自动质谱解卷积定性系统与结合文献定性,环已酮为内标定量。结果:在川芎-香附药对挥发油中共鉴定出66种化学成分,含量较高的物质分别为α-香附烯、β-芹子烯、香附烯酮、α-香附酮及(z)-蒿苯内酯。结论:川芎-香附药对挥发性成分谱全部由单味中药川芎与香附化学成分构成,药对中未发现新增加的挥发性成分。     

明目疏脉片质量标准研究

建立明目疏脉片质量标准。采用薄层色谱法对蒺藜、枸杞、丹参、当归和川芎进行鉴别;采用高效液相色谱法测定赤芍中芍药苷的含量,色谱柱为Thermo C18(150×4.6mm,5μm),流动相为乙腈-0.3%磷酸水溶液(10.8∶89.2 V/V),检测波长为230 nm,柱温为30℃,流速为1.0 mL/min。蒺藜、枸杞、丹参、当归和川芎的TLC特征斑点分离清晰,阴性无干扰。芍药苷在0.0768~0.768μg范围内线性关系良好(r=0.9998);供试品溶液在24 h内稳定,平均加样回收率为98.12%,RSD=1.48%(n=6)。所建标准准确可靠、重复性好,可用于控制明目疏脉片的质量。     

以咖啡酸和阿魏酸为指标从不同炮制因素的角度探究川芎酒炙机理

从加热因素、炒制时间和炮制辅料三方面入手,以咖啡酸和阿魏酸为指标来探究川芎的酒炙机理。通过改变不同炮制因素后川芎中咖啡酸和阿魏酸的含量测定,发现黄酒闷润后的川芎经过加热炒制(炒制5～30 min),其咖啡酸和阿魏酸含量均比不经过炒制者高,且随炒制时间的延长,咖啡酸和阿魏酸的含量变化趋势一致,均为先增高后降低,在炒制20 min时达到最大值。用黄酒和水闷润后进行加热炮制两种成分含量均比用不同浓度乙醇闷润的含量高。与以往的理论不同,咖啡酸和阿魏酸含量增高可能并不是因为黄酒中乙醇的存在而增加了溶出。     

苗药土党参化学成分定性研究

对苗药土党参化学成分进行定性研究。采用化学反应鉴别法对土党参药材的水提取液、乙醇提取液和石油醚提取液进行系统化学预实验,结果表明土党参可能含有多糖、黄酮、皂苷、甾体、有机酸、香豆素、挥发油、油脂等多类化合物;同时,以党参炔苷为对照品,采用薄层色谱法(TLC)进行药材定性鉴别。本研究为进一步探索土党参药材的生物活性成分提供实验基础;所建立的土党参薄层色谱定性鉴别方法为土党参药材鉴别提供参考依据。     

菊花薄层色谱鉴别方法的研究

为了改善《中国药典》中菊花薄层色谱鉴别方法以便控制药材的内在质量,采用薄层色谱法对菊花原料进行定性鉴别研究,将菊花薄层色谱鉴别中的以甲苯-乙酸乙酯-甲酸-冰醋酸-水(1∶15∶1∶1∶2)的上层溶液为展开剂改为"乙酸丁酯∶甲酸∶水(8∶2.5∶2.5)"的上层溶液为展开剂,结果表明薄层色谱上具有鉴别特征,色谱斑点清晰,专属性强;该方法操作简便,稳定性、重现性均很好。该方法可以用于菊花原料的薄层鉴别。     

川芎提取物挥发性成分分析及在卷烟中的应用研究

采用超临界流体萃取得到川芎提取物,平均收率为6.86％。利用毛细管气相色谱-质谱联用仪对川芎提取物成分分离并鉴定出47种化学成分.用峰面积归一化法测定各种成分的质量分数,结果表明超临界CO2川芎提取物的主要成分为：3-丁基苯酞、3-丁叉苯酞、棕榈酸、亚油酸、川芎内酯等。卷烟加香实验表明：川芎提取物能有效掩盖卷烟杂气,使烟气柔和、香气细腻,可明显提高卷烟质量。     

川芎血清药物化学成分研究

通过药物化学手段研究川芎的血清移行成分,以期为本药品的有效成分鉴定、提取及用药提供指导。制备对照组溶液及川芎灌胃液,建立大鼠模型,灌胃后提取血清,建立HPLC指纹图谱,并鉴定血中移行成分。本次共检出11个成分,其中4个成分属于血清,川芎提取液灌胃后从血中发现了7个入血成分,其中4个为代谢产物,3个为原型成分。川芎入血成分主要为川芎嗪和阿魏酸,可为阐明川芎药理作用及其质量控制提供依据。     

川芎化学成分及药理作用研究新进展

川芎作为祖国传统中药材,素因其有效的化学成分及广泛的药理作用而闻名于世。川芎所含有的多种化学成分分别在抗炎、镇痛、抗血栓形成、促血管舒张、抗哮喘、抗呼吸抑制、抗纤维化、抗阻塞性疾病及抗肿瘤等方面产生了积极的影响。在这些有效成分中,以苯酞类化合物、川芎嗪以及阿魏酸的作用最为广泛且效力更强,洋川芎内酯以及藁本内酯等亦发挥了积极地作用。目前,研究者们对川芎中有效化学成分在临床应用中的作用机制的研究尚未深入,其所具有的药理作用亦需要更进一步的探究。本文对川芎的化学成分及其药理作用的研究新进展进行综述与总结,以期为今后更进一步探索川芎的药用前景提供科学依据及理论参考。     

复方王不留行片的薄层色谱鉴别研究

目的建立复方王不留行片的薄层色谱鉴别方法,为其质量控制提供实验依据。方法采用薄层色谱鉴别法鉴别处方中的主要药味。结果处方中的王不留行主药的薄层色谱具有明显鉴别特征。结论薄层色谱鉴别方法简便可靠,专属性、重现性好,可作为复方王不留行片的质量控制指标。     

黄菊提取物分析方法研究

采用TLC法对黄菊提取物中野菊花进行定性鉴别,采用HPLC法测定黄菊提取物中的黄芩苷并进行水分、水中不溶物的测定。TLC定性检出野菊花,斑点清晰,分离度好,阴性对照无干扰;黄芩苷在1.862~186.195μg·mL~([-1])(r=0.9997)与峰面积均呈现良好的线性关系,平均回收率为102.08%,RSD(n=9)为1.57%。     

Extraction of ferulic acid from oil palm pressed fiber by a choline chloride based deep eutectic solvent

Results on the extraction of ferulic acid from palm pressed fiber using deep eutectic solvent (DES) of choline chloride-acetic acid (ChCl-AA) and choline chloride-citric acid (ChCl-CA) are reported. Acetic acid was found to be a better hydrogen bond donor to choline chloride than citric acid for the extraction of ferulic acid. Influence of water content in both DES was investigated whereby ChCl-AA and ChCl-CA experienced a drop in viscosity from 9.678 to 1.429 and 22.658 ± 1.655 mm²/s, respectively as the water content in the DES increased from 0 to 50 wt%. The drop in viscosity contributed to higher extraction efficiency in which 41,155 ± 940 mg/kg ferulic acid was obtained after 6 h reflux when ChCl-AA with 30 wt% water was used for the extraction compared to 30,940 ± 621 mg/kg when neat ChCl-AA was used. Further increase in water content in the DES however, did not lead to higher extraction efficiency. Although viscosity of the DES could be improved with the addition of water, there is a threshold where the DES could tolerate the presence of water without changing its solvent behavior. Surface response model revealed that interaction between heating duration and water content in DES, as well as second order effect of both heating duration and water content in DES played important roles in the extraction of ferulic acid from oil palm pressed fiber. The optimum condition for extraction of ferulic acid from palm pressed fiber was heating for 6 h with DES containing 30 wt% water.     

阿魏酸苦参碱盐的合成

目的：通过对苦参碱的结构进行修饰,寻求疗效更好、毒副作用更小的化合物。方法：以苦参碱为原料,利用其碱性,通过酸碱成盐合成阿魏酸苦参碱盐。结论：合成得到了目标化合物,产率为90．5％,并通过TLC、IR、MS等方法对其结构进行了初步验证。     

降糖胶囊薄层鉴别质量标准研究

按照新的药品注册管理办法要求,研究了降糖胶囊的薄层鉴别方法。考察了供试品前处理工艺,筛选薄层鉴别的色谱条件,建立了降糖胶囊中红参、黄芪、淫羊藿的薄层色谱方法。该方法简便,专属性强,重现性好,可用于降糖胶囊的定性质量控制。     

Radical Scavenging Activity of Lipophilized Products from Lipase-Catalyzed Transesterification of Triolein with Cinnamic and Ferulic Acids

Lipase-catalyzed transesterification of triolein with cinnamic and ferulic acids using an immobilized lipase from Candida antarctica (E.C. 3.1.1.3) was conducted to evaluate the antioxidant activity of the lipophilized products as model systems for enhanced protection of unsaturated oil. The lipophilized products were identified using ESI-MS. Free radical scavenging activity was determined using the DPPH radical method. The polarity of the solvents proved important in determining the radical scavenging activity of the substrates. Ferulic acid showed much higher radical scavenging activity than cinnamic acid, which has limited activity. The esterification of cinnamic acid and ferulic acid with triolein resulted in significant increase and decrease in the radical scavenging activity, respectively. These opposite effects were due to the effect of addition of electron-donating alkyl groups on the predominant mechanism of reaction (hydrogen atom transfer or electron transfer) of a species with DPPH. The effect of esterification of cinnamic acid was confirmed using ethyl cinnamate which greatly enhances the radical scavenging activity. Although, compared to the lipophilized cinnamic acid product, the activity was lower. The radical scavenging activity of the main component isolated from lipophilized cinnamic acid product using solid phase extraction, monocinnamoyl dioleoyl glycerol, was as good as the unseparated mixture of lipophilized product. Based on the ratio of a substrate to DPPH concentration, lipophilized ferulic acid was a much more efficient radical scavenger than lipophilized cinnamic acid.     

反相高效液相色谱法测定川楝子中阿魏酸含量

建立测定川楝子中阿魏酸含量的高效液相色谱法。采用VP-ODS C18（250 mm×4.6 mm,5μm）色谱分析柱;流动相为甲醇-1%冰醋酸（25：75）;检测波长：320 nm;流速：0.8 mL/min。结果阿魏酸进样量在0.25~2.50μg范围内与峰面积呈良好的线性关系（r=0.999 6）,平均加样回收率为99.38%,RSD=1.18%（n=6）。该方法简便、准确、可靠,可作为川楝子中阿魏酸的定量分析方法。     

气相色谱法测定牙膏中二甘醇含量

建立了气相色谱法测定牙膏中二甘醇含量的方法。试样用30 mL无水乙醇35℃超声提取30 min,取上清液用0.45μm有机滤膜过滤后直接进行气相色谱分析。测定中选用HP-INNOWAX毛细管柱,氢火焰离子检测器,程序升温,外标法进行定量。二甘醇在10～10 000μg/mL浓度内线性关系良好(r=0.999 9);平均回收率为92.8%(RSD=0.32%,n=9)。采用该方法对23个品牌的牙膏进行了测定,结果表明该方法能对二甘醇准确定量,具有线性范围宽、操作简单、快速实用等特点,对工厂生产中杜绝二甘醇的出现具有一定的现实指导意义。     

大鲵肽在牙膏中的应用研究

采用酶法从人工饲养大鲵肉中提取得到大鲵肽,利用串联飞行时间质谱仪(MALDI-TOF/TOF)测定其分子量主要为1 422,1 521,1 746,1 828和1 879,均小于2 000,酶解产物大鲵肽为低聚肽。将提取到的大鲵肽应用到牙膏中,应用自由基清除活性评价方法研究了大鲵肽牙膏的抗氧化活性。结果表明,牙膏中添加质量分数为0.1%的大鲵肽可达到较好的抗氧化效果,其牙膏水溶液具有清除DPPH自由基、羟基自由基(·OH)、超氧阴离子自由基以及ABTS自由基的能力。     

Production of vanillin from wheat bran hydrolyzates via microbial bioconversion

BACKGROUND: Wheat bran contains a large amount of ferulic acid, which can be released through enzymatic hydrolysis and bioconverted into vanillin. A previous study has shown that ferulic acid purification from bran carbohydrates with the Amberlite^® IRA 95 resin allowed an increased vanillin molar yield. In this work, alternative ferulic acid recovery methods were proposed and the possibility of exploiting the residual carbohydrate‐rich water phase was explored. RESULTS: Ferulic acid was recovered from crude wheat bran hydrolyzate by: (i) a hydrophobic sorbent cartridge (ISOLUTE ENV^+®): (ii) ethyl acetate extraction; and (iii) the resin previously employed. The highest recovery percentage (95%) was obtained with ISOLUTE ENV^+®, which also allowed an interesting vanillin molar yield from ferulic acid bioconversion (75% from 0.5 mmol L^?1 ferulic acid). The residual water phase was a good growth substrate for the microorganism operating the bioconversion. Cells grown on this matrix could efficiently bioconvert the recovered ferulic acid to vanillin CONCLUSION: The possibility of efficiently recovering ferulic acid from wheat bran hydrolyzates, bioconverting it into vanillin, and valorizing the sugar‐rich exhausted water fraction was demonstrated in this work. The approach allowed the production of a value‐added fine‐chemical from a food‐industry by‐product. Copyright © 2009 Society of Chemical Industry