浓缩当归丸的提取工艺研究

采用索氏提取法提取浓缩当归丸的有效成分阿魏酸，同时用正交分析法对提取溶剂种类、用量及提取时间进行考察，最后以高效液相色谱法(HPLC)测定阿魏酸的含量，从而筛选出最佳提取工艺．结果显示：选用60mLV甲醇：V甲酸=95：5的混合液作为提取溶剂．预先浸泡24h，再索氏提取3h，得到浓缩当归丸的有效成分阿魏酸的含量最高．     

高效液相色谱与质谱联用分析测定川芎中有效成分阿魏酸与藁本内酯

采用HPLC-MS系统地研究了中药川芎有效成分阿魏酸(ferykuc acid)和藁本内酯(liguatilide)的定量分析方法。利用制备色谱制备了藁本内酯对照品,并对其进行了紫外光谱、质谱、红外光谱等结构鉴定。分别考察了水、甲醇、乙醇、95％乙醇4种溶剂以及提取时间对川芎中阿魏酸和藁本内酯提取量的影响。结果表明：水是阿魏酸的最佳提取溶剂,提取时间45min为宜;乙醇是适合提取藁本内酯的溶剂,提取时间75min为宜。以外标法对市售川芎中的阿魏酸与藁本内酯进行了定量分析,二者含量分别是0．15％(m／m)和0．82％(m/m)。     

以氢化阿魏酸为假模板制备的印迹聚合物对阿魏酸的识别

以氢化阿魏酸为假模板分子(dummy template),4-乙烯基吡啶为功能单体,通过自组装技术在乙腈中制备了对阿魏酸具有良好识别能力的印迹聚合物.采用平衡吸附法表征了聚合物在不同吸附条件下对阿魏酸的吸附特性及分子识别性能,并用紫外光谱滴定法和Scachard结合模型研究了聚合物的印迹机理和识别机理.研究表明,该聚合物对阿魏酸的识别能力甚至高于氢化阿魏酸,而且在50%的水溶液仍能有效识别阿魏酸.进一步将该聚合物用于川芎水提液中阿魏酸的提取分离,获得较好结果,显示该聚合物具有直接作为传统中药中阿魏酸分离提取材料的潜能.     

以氢化阿魏酸为假模板制备的印迹聚合物对阿魏酸的识别

以氧化阿魏酸为假模板分子（dummy template），4-乙烯基吡啶为功能单体，通过自组装技术在乙腈中制备了对阿魏酸具有良好识别能力的印迹聚合物。采用平衡吸附法表征了聚合物在不同吸附条件下对阿魏酸的吸附特性及分子识别性能，并用紫外光谱滴定法和Scachard结合模型研究了聚合物的印迹机理和识别机理。研究表明，该聚合物对阿魏酸的识别能力甚至高于氧化阿魏酸，而且在50％的水溶液仍能有效识别阿魏酸。进一步将该聚合物用于川芎水提液中阿魏酸的提取分离，获得较好结果，显示该聚合物具有直接作为传统中药中阿魏酸分离提取材料的潜能。     

超临界CO2萃取、HPLC法测定川芎中的阿魏酸

采用超临界CO2萃取法提取川芎中的阿魏酸,通过试验确定了最佳超临界萃取条件,萃取罐的温度为60℃、萃取压力为35 MPa、萃取时间为2 h。以甲醇-水-冰乙酸(体积比为30∶70∶0.2)为流动相,用HPLC法测定川芎中的阿魏酸,回收率为92.3%~103.4%,相对标准偏差为2.45%(n=6)。     

毛细管电泳同时分离测定阿魏酸、异阿魏酸的研究

建立了同时分离测定阿魏酸、异阿魏酸的毛细管电泳(CZE)新方法。以20 mmol/L硼砂为背景电解质,体积分数15%异丙醇为有机改性剂,分离电压为20 kV,在219 nm波长下紫外检测。对硼砂浓度、有机溶剂体积分数、分离电压等因素对分离的影响做了系统的研究,最后确立了阿魏酸、异阿魏酸的最佳分离条件。阿魏酸、异阿魏酸分别在2.40~24.0μg/mL、1.80~18.0μg/mL范围内线性关系良好(r=0.9995和r=0.9991),回收率分别为96.61%~101.9%,98.80%~101.8%。方法已用于升麻中阿魏酸、异阿魏酸的测定。     

黔产野生藤梨根的化学成分研究

对贵州省安顺市紫云县产的野生藤梨根的化学成分进行研究。利用稀乙醇提取液蒸干,甲醇溶解等对其化学成分进行提取,利用高效液相色谱(HPLC)和薄层色谱(TLC)对其成分进行分析。野生藤梨根中含有阿魏酸、齐墩果酸、熊果酸、棕榈酸、表儿茶素、大黄素、槲皮素等,用HPLC对野生藤梨根中的阿魏酸、表儿茶素进行了鉴定,用TLC对野生藤梨根中的大黄素,齐墩果酸、熊果酸、棕榈酸、槲皮素进行了鉴定。     

反相高效液相色谱法测定补钙保健品中的维生素D_3

 用氯仿作提取剂直接提取补钙保健品中的维生素Ｄ３,提取液经浓缩后进行高效液相色谱分析,并对皂化和直接提取的样品中维生素Ｄ３的含量进行了比较。采用μ－ＢｏｎｄａｐａｋＣ１８作分离柱,甲醇－水（８７１３）作流动相,检测波长为２６４ｎｍ,回收率为９５．６３％。     

反相高效液相色谱法测定川芎饮片、实验大鼠血清和脑匀浆中的阿魏酸

 用反相高效液相色谱法测定了川芎饮片、实验大鼠血清和脑匀浆中的阿魏酸。分离柱为Nova Pak C18(3 9mmi.d .× 15 0mm) ,流动相为甲醇 水 乙酸 (体积比为 35∶6 5∶0 5 ) ,在 32 0nm波长下检测 ,用外标法定量。阿魏酸在 0 85mg/L～ 4 0 0mg/L范围内有良好的线性关系 ,线性相关系数为0 9990 4。阿魏酸的加标回收率为 95 %～ 10 2 %。     

反相高效液相色谱法测定补钙保健品中的维生素D_3

用氯仿作提取剂直接提取补钙保健品中的维生素Ｄ３，提取液经浓缩后进行高效液相色谱分析，并对皂化和直接提取的样品中维生素Ｄ３的含量进行了比较。采用μ－ＢｏｎｄａｐａｋＣ１８作分离柱，甲醇－水（８７１３）作流动相，检测波长为２６４ｎｍ，回收率为９５．６３％。     

KMnO4-乙二醛化学发光体系测定阿魏酸

酸性介质下,KMnO4氧化阿魏酸产生化学发光,乙二醛对该体系有增敏作用。结合流动注射技术,建立了测定阿魏酸的流动注射化学发光新方法。该方法线性范围为1.0×10-7～2.0×10-5mol/L,检出限为1.0×10-8mol/L,对1.0×10-6mol/L的阿魏酸平行测定11次,相对标准偏差为2.8%。该法用于太太美容口服液中阿魏酸的测定,结果令人满意。     

Chemiluminescence determination of ferulic acid by flow-injection analysis using cerium(IV) sensitized by rhodamine 6G

A simple, sensitive and rapid flow-injection chemiluminescence method has been developed for the determination of ferulic acid based on the chemiluminescence reaction of ferulic acid with rhodamine 6G and ceric sulfate in sulphuric acid medium. Strong chemiluminescence signal was observed when ferulic acid was injected into the acidic ceric sulfate solution in a flow-cell. The present method allowed the determination of ferulic acid in the concentration range of 8.0x10(-6) to 1.0x10(-4)moll(-1) and the detection limit for ferulic acid was 8.7x10(-9)moll(-1). The relative standard deviation was 2.4% for 10 replicate analyses of 1.0x10(-5)moll(-1) ferulic acid. The proposed method was applied to the determination of ferulic acid in Taita Beauty Essence samples with satisfactory results.     

Assay of free ferulic acid and total ferulic acid for quality assessment of Angelica sinensis

Activity of Chinese Danggui (DG), the processed root of Angelica sinensis (Oliv.) Diels, is linked to the ferulic acid content but the stability of ferulic acid during extraction for medicinal use is not known. The stabilities of ferulic acid and coniferyl ferulate were evaluated in the extracts of DG using a variety of extraction solvents. These included various combinations and proportions of methanol, water, formic acid, 1 M aqueous hydrochloric acid and 2% sodium hydrogen carbonate (NaHCO3) in water. Coniferyl ferulate was found liable to hydrolyze into ferulic acid in neutral, strongly acidic and basic solvents, where heat and water could facilitate this hydrolysis. However, the hydrolysis was relatively resisted in weakly organic acid. Based on the stability evaluation, two new terms, namely: free ferulic acid and total ferulic acid, were suggested and defined. Free ferulic acid refers to the natural content of ferulic acid in herbs. Total ferulic acid means the sum of free ferulic acid plus the amount of related hydrolyzed components. Meanwhile, the high-performance liquid chromatographic (HPLC) method was developed to assay free ferulic acid and total ferulic acid in DG using methanol-formic acid (95:5) and methanol-2% NaHCO3 in water (95:5) as extraction solvents, respectively. Ten DG samples were investigated on their contents of free and total ferulic acid. The results indicated that the amount variety of free ferulic acid was larger than that of their counterparts, and the ratio of total ferulic acid to free ferulic acid was 4.07 +/- 2.73 (mean +/- SD, n = 10). The chemical assay of DG using total ferulic acid content would be a better choice to assess the herbal quality and was recommended.     

Permanganate-based chemiluminescence analysis of ferulic acid using flow injection.

A simple, sensitive and rapid flow-injection chemiluminescence method has been developed for the determination of ferulic acid based on the chemiluminescence reaction of ferulic acid with potassium permanganate in a nitric acid medium. A strong chemiluminescence signal was observed when ferulic acid was injected into an acidic potassium permanganate solution in a flow-cell. The present method allowed the determination of ferulic acid in the concentration range of 6.0 x 10(-6) to 2.0 x 10(-4) mol l(-1); the detection limit (3sigma) for ferulic acid was 9.6 x 10(-8) mol l(-1). The relative standard deviation was 1.0% for 11 replicate analyses of 2.0 x 10(-4) mol l(-1) ferulic acid. The proposed method was applied to the determination of ferulic acid in real samples with satisfactory results. Moreover, the reaction mechanism of the chemiluminescence system was primarily considered.     

Separation and determination of three phenylpropanoids in the traditional Chinese medicine and its preparations by capillary electrophoresis

Three phenylpropanoids (ferulic acid, chlorogenic acid, and caffeic acid) are simultaneously separated and determined within 13 min by a new capillary electrophoresis method using 15 mmol/L sodium borate (pH 8.71) as run buffer. The optimum conditions for the separation as well as the analytical characteristics, such as the calibration graph and limit of detection (LOD) for the determination of these three compounds, are studied. The linear range for the determination of ferulic, chlorogenic, and caffeic acid is 5.0 approximately 70.0, 8.0 approximately 112.0, and 9.0 approximately 64.0 microg/mL, with the LOD as 1.5, 2.25, and 6.0 microg/mL, respectively. The method, which is very simple, rapid, and of requisite sensitivity and reproduction, is satisfactorily used for the separation and determination not only of ferulic, chlorogenic, and caffeic acid in Cimicifuga foelida Li and its preparation (Yin-huang-han-pian), but also of ferulic acid and chlorogenic acid in Ligusticum chuanxiong hort. and Angelica sinensis (Oliv.) Diels.     

Simultaneous determination of hydroxysafflor yellow A and ferulic acid in rat plasma after oral administration of the co-extractum of Rhizoma chuanxiong and Flos Carthami by HPLC-diode array detector

A simple, rapid and accurate HPLC method has been developed for simultaneous determination of hydroxysafflor yellow A and ferulic acid in rat plasma after oral administration of the co-extractum of Rhizoma chuanxiong and Flos Carthami. Plasma samples were deproteinized with 6% perchloric acid, and riboflavin was used as internal standard. The supernatant after centrifuge was injected into a Shimadzu C(18) (150 x 4.6 mm, i.d. 5 microm) column. Gradient elution for A:B (0 min, 90:10; 25 min, 70:30; 27 min, stop) was applied. The mobile phase was composed of 0.022 mol/L potassium dihydrogen phosphate solutions, adjusted to pH 3.0 with phosphoric acid for pump A, and 90% (v/v) acetonitrile for pump B. The assay was shown to be linear over the range 0.046-4.6 microg/mL (r(2) = 0.9995) for hydroxysafflor yellow A and 0.037-3.7 microg/mL (r(2) = 0.9998) for ferulic acid. Mean recovery was 97.5% for hydroxysafflor yellow A and 83.6% for ferulic acid. Both of the intra-day and inter-day precisions were 相似文献   

高效液相色谱-串联质谱法同时测定水溶性迷迭香提取物中迷迭香酸、阿魏酸和咖啡酸的含量

本文建立了一种同时快速测定水溶性迷迭香提取物中迷迭香酸、阿魏酸和咖啡酸含量的高效液相色谱-串联质谱(HPLC/MS/MS)分析方法。以甲醇和0.1%乙酸铵溶液为HPLC的流动相;MS/MS使用多反应监测(MRM)扫描方式,在3 min内可完成迷迭香酸、阿魏酸和咖啡酸三种化合物的分离分析。上述三种分析物在5~500 ng/mL范围内线性良好(r>0.999);检出限均低于5.0 ng/mL。本法操作简便、分析速度快、灵敏度高,可用于水溶性迷迭香提取物中迷迭香酸、阿魏酸和咖啡酸含量的测定。     

Routine analysis of ascorbic acid in citrus juice using capillary electrophoresis.

A procedure to monitor citrus juice samples was established to quantitate vitamin C by capillary electrophoresis using a previously developed method. Dilution and filtration were the only preparation requirements and separation was achieved with an uncoated capillary using a 35mM sodium borate buffer (pH 9.3) containing 5% (v/v) acetonitrile at 21 kV and 23 degrees C. Detection was performed by high speed scanning between 200 and 360 nm. From the multiwave length scan, the electropherogram at 270 nm was extracted and used to quantitate ascorbic acid. The ascorbic acid concentration was calculated with an internal standard method, with ferulic acid as internal standard. The level of ascorbic acid during analysis was stabilized with ethylenediaminetetraacetic acid and dithiothreitol was used to reduce dehydroascorbic acid to ascorbic acid to estimate the total vitamin C level. Results were similar to those obtained by liquid chromatography and the method is now used to determine routinely the level of ascorbic acid in citrus juices.     

碳糊电极阴极溶出伏安法测定当归中阿魏酸

采用碳糊电极作工作电极,阴极溶出伏安法对阿魏酸进行测定。在0.05mol.L-1盐酸溶液中,当有0.04mmol.L-1氯化钠溶液,0.004g.L-1十二烷基硫酸钠溶液存在时,1.1V(vs.SCE)富集180s,以100mV.s-1扫描速率从1.0V扫描至0V。阿魏酸在碳糊电极上于0.46V处产生一灵敏的阴极溶出伏安峰,峰电流与阿魏酸浓度在2.2×10-7～1.1×10-5 mol.L-1范围内呈线性关系,检出限(3S/N)为4.0×10-8 mol.L-1。初步探讨了阿魏酸的电化学性质,此方法用于测定当归中阿魏酸的含量,并以此样品为基体做回收试验,测得回收率在104.0%～109.1%之间,测定值的相对标准偏差(n=6)在2.6%～5.3%之间。