七叶莲总皂苷定量分析方法及其提取工艺研究

以齐墩果酸为对照品,建立了比色法测定七叶莲总皂苷含量的方法;以总皂苷得率为指标,采用正交试验法对七叶莲总皂苷提取工艺进行了优化.结果表明:在比色法定量分析时,以5%香草醛冰醋酸溶液-高氯酸为显色剂,70℃加热15min显色后,选择546nm为测定波长,在40min内,测量结果稳定,总皂苷质量浓度在0.002~0.02g/L范围内呈良好的线性关系(r=0.99933);平均加样回收率为101.2%,相对标准偏差(RSD)为0.86%(n=6).在提取过程中,优化的工艺参数为:以50%(体积分数)乙醇为溶剂,控制固液比1∶15(g∶mL),80℃水浴提取2次,每次120min,此条件下总皂苷得率1.217%.     

希腊海岸松叶中聚戊烯醇含量与化学结构分析

利用HPLC与聚戊烯醇对照品保留时间对照的定性方法,确定海岸松叶中聚戊烯醇的异戊烯基单元数为14~20;利用1H NMR和13C NMR确定海岸松聚戊烯醇化学结构为ω-trans2-cisn-OH构型。采用Kromasil C18 ODS-1(150 mm×4.6 mm,5μm)色谱柱,以甲醇-异丙醇(体积比9∶16)为流动相,流速为0.50 mL/min,检测波长为210 nm,柱温为25℃,PDA检测器等色谱条件,测定海岸松叶聚戊烯醇在1.10~12.10μg范围内线性良好(r=0.996 3),平均回收率为98.21%,RSD为2.27%(n=6),海岸松干叶中聚戊烯醇含量为0.33%。     

HPLC法同时测定不同品种、产地、部位松树中莽草酸的含量北大核心

研究采用HPLC法同时测定不同品种、产地、部位松树中莽草酸的含量,以期为开发莽草酸资源提供参考。色谱柱为Agilent Eclipse Plus C_(18)(250 mm×4.6 mm,5 m),流动相为甲醇/0.1%磷酸水溶液(体积比为10∶90),检测波长为217 nm,柱温为30℃。采用直观分析结合聚类分析对不同品种、产地、部位松树中莽草酸含量的差异性进行统计分析。结果表明:莽草酸的线性关系良好(r=0.9995),平均加样回收率为100.4%(n=6),RSD为1.71%。6种松树中的莽草酸含量由高到低依次为雪松、华山松、白皮松、油松、樟子松、落叶松。其中,天水雪松松针中的莽草酸含量最高,达31.47 mg/g。通过聚类分析发现,6种松树中的莽草酸可划分为3类。     

沙棘籽油中VE含量测定方法

用高效液相色谱法测定沙棘籽油中VE含量,并对方法进行了考查。波长292 nm处,VE进样浓度在0.3 m g/mL~1.0 m g/mL范围内,呈现良好线性,相关系数r=0.999 9,回收率97.47%,相对偏差2.22%,表明检测方法准确,结果可靠。     

紫椴花多糖的超声提取最佳条件和含量测定

设置7个萃取温度（25,35,45,55,65,75,85。C）和萃取时间（30,40,50,60,70,80,90min）来选择超声提取紫椴花中多糖的最佳提取温度和提取时间。利用分光光度法对紫椴花中的多糖含量进行了分离和测定。结果表明：最佳提取条件为提取温度为75℃,提取时间为52min。经蒽酮—硫酸显色,于580nm处测定,其多糖的含量为9．74％,RSD=0．47％（n=3）。此测定方法简便,样品溶液在4h内显色稳定,重现性较好,平均回收率为99．48％±1．01％,RSD=0．112％（n=3）。     

杜仲叶酸性多糖提取分离及含量测定

研究杜仲叶酸性多糖的提取分离工艺及其含量测定的简便方法.结果表明,以提取过药用有效成分后的杜仲叶为原料提取酸性多糖的较佳工艺条件是:1.0%的碱水在100 ℃下提取2次,每次2 h;提取液经大孔吸附树脂处理,多次醇沉等步骤分离的酸性多糖含量可达到41.46%.采用DNS法测定杜仲叶酸性多糖含量时水解时间控制在15～20 min,显色反应为10 min,检测波长为492 nm;在试验条件下,葡萄糖浓度在0.20～0.60 mg·mL-1范围内显色灵敏、稳定,线性关系良好;用该法测定杜仲叶渣酸性多糖含量时加样回收率为98.30%,RSD为1.76%;显色溶液在2 h内吸光度值比较稳定,能够完全满足测定工作要求,可以作为实验室测定多糖含量的简便、快捷、有效的方法.     

富贵菜茎及不同发育时期叶总黄酮含量的比较

测定大田栽培富贵菜总黄酮的含量。结果:芦丁在0.00~51.352μg/mL(r=0.999 4)范围内线性关系良好,平均回收率为98.36%,RSD=1.20%(n=5)。所测样品总黄酮的含量中叶的含量高于茎。嫩叶的最高,为3.338%;其次为成熟叶1.813%;老叶为1.338%,茎最低,为0.3%。     

HPLC法同时测定闽产圆齿野鸦椿中两种色原酮碳苷的含量

建立了HPLC同时测定圆齿野鸦椿中两个成分5,7-二羟基-2-甲基-色原酮-8-C-β-D-葡萄糖苷(A)和5,7-二羟基-2-甲基-色原酮-6-C-β-D-葡萄糖苷(B)的方法,并测定了这两个成分在闽产圆齿野鸦椿枝条、叶片、果皮和种子中的含量。结果表明:HPLC测试条件为色谱柱DikmaDiamonsil C18柱(250 mm×4.6 mm,5μm),流动相甲醇/水(25∶75,体积比),等度洗脱,流速为1.0 mL/min;检测波长256 nm,柱温30℃,检测时间15 min时,化合物A和B分别在2.000 2～20.002 0μg和2.001 6～20.016 0μg范围内线性关系良好(r=0.999 9),平均加样回收率分别为98.42%和99.77%,RSD均小于1.00%(n=6)。HPLC法快速简便、重复性和稳定性好、结果准确可靠,可为今后圆齿野鸦椿在药用植物资源开发应用方面提供依据。     

箬竹叶总黄酮含量的测定

用N aNO2-A l(NO3)3比色法在510 nm处测定箬竹叶乙醇提取液吸光度,以芦丁为标准品,建立了芦丁标准工作曲线回归方程:c(m g.L-1)=95.43A-0.735 9,相关系数r=0.999 8.通过稳定性实验确定了显色后溶液吸光度的测定时间;通过正交实验确定了水浴提取和超声提取的最佳条件,并实验了提取次数对箬竹叶总黄酮含量的影响,测得箬竹叶总黄酮含量为1.38%;通过回收率实验,表明此法测定箬竹叶总黄酮含量准确可靠.     

芜湖产地牡丹皮的质量分析

利用HPLC法测定芜湖产地牡丹皮中丹皮酚的含量。采用HPLC法,色谱柱为Agilent Eclipse C18(4.6mm×150mm,5μm)。流动相为乙腈-0.3%磷酸水溶液,梯度洗脱,检测波长274nm,柱温30℃,流速1.0mL/min。丹皮酚在0.0325～0.52μg范围内线性关系良好(R=0.9996),平均回收率为102.51%,RSD为1.26%。结果表明,芜湖产地牡丹皮中有效成分丹皮酚的含量高于《中国药典》的规定,平均含量为1.91%。     

野生半夏中β-谷甾醇含量的测定

笔者用紫外分光光度法测定了半夏中β-谷甾醇的含量。以浓硫酸为显色剂,在416nm处测定β-谷甾醇的吸光度。结果表明:β-谷甾醇浓度在10～50μg/mL范围内呈良好线性关系,r=0.9983,β-谷甾醇的含量为0.1612%。与其他地区相比,含量较高。     

山杏叶桦木酸、齐墩果酸和熊果酸的研究

我国山杏资源十分丰富,是绿化荒山的优良树种。采用HydersirBDSC18色谱柱（150×4．6mm,5μm）,流动相体积比为90：10的0．3‰硫酸甲醇溶液一3‰硫酸水溶液,检测波长210nm,建立了山杏叶中三萜酸测定的高效液相色谱法。结果表明：桦木酸、齐墩果酸与熊果酸的浓度在30～2000μg／mL（r桦=0．9971,r齐=0．9986,r熊=0．9978）范围内与色谱峰面积呈良好线性关系;平均加标回收率分别为99．9％、101．1％和98．9％。以山杏叶为材料,采用高效液相色谱法和紫外可见分光光度法分别对山杏叶中的三萜酸成分进行分析,结果表明,山杏叶富含三萜酸,落叶期山杏叶中总三萜酸（17078#g／g）、桦木酸（1842μg／g）、齐墩果酸（2536μg／g）和熊果酸（5706μg／g）含量均高于非落叶期。本研究首次建立了山杏叶中桦木酸、齐墩果酸和熊果酸同时测定的反向高效液相色谱法（HPLC）,发现落叶期山杏叶富含三萜酸,为山杏叶综合开发利用提供了基础数据。     

Rapid spectroscopic separation of three Canadian softwoods

Near Infrared (NIR) and Fluorescence (FS) spectroscopy were investigated for their ability to rapidly separate three Canadian softwoods: balsam fir, western hemlock, and white spruce. NIR and FS spectral data were used to develop classification models using soft independent modeling of class analogies (SIMCA) method. For each wood species, spectra of 90 wood specimens were collected over a wavelength window of 800–2,500?nm for NIR spectral data and a wavelength range of 380–540 and 380–705?nm for FS spectral data. Raw spectra and first-derivative-transformed spectra were used to develop NIR calibration models to separate the three wood species using the wavelength ranges, 800–2,500, 1,100–2,200, and 1,300–2,000?nm, by the SIMCA method. Similarly, FS raw spectral data were also used to develop FS calibrations using wavelength ranges of 380–540 and 380–705?nm. Principal component analysis models were made for each class from the calibration set consisting of 65 specimens of each of the three wood species. Specimens not present in the calibration set (27 specimens of each wood species) were tested for classification according to the SIMCA method at a 5 and 25% significance level. Type I error associated with the models developed with NIR spectral data ranged from 0 to 19 and 0 to 52% for the 5 and 25% significance levels, respectively, while type II error ranged from 2 to 50 and 0 to 19%, respectively. When tested at a 5% significance level, there was no significant improvement in NIR models developed with first-derivative-transformed spectra over models developed with raw spectra. Type I error associated with the models developed with Fluorescence spectral data ranged from 0 to 4 and 7 to 30% for the 5 and 25% significance levels, respectively, while type II error ranged from 1 to 9 and 0 to 1%, respectively. There were no significant differences in performance of FS models developed with spectra using wavelength ranges of 380–540 and 380–705?nm.     

半夏不同采收期总生物碱含量的动态变化研究

采用氯仿提取 ,依据酸性染料比色法的原理 ,在 41 7nm波长下测定半夏中总生物碱含量 ,进行方差分析。结果表明 :获得良好的线性关系 (r=0 9989)和回收率 ( 1 0 0 1 %) ,RSD为2 3%。半夏不同采收期总生物碱含量差异显著 (F =2 31 3,P <0 0 5 )。结论 :测定方法简单快速 ;半夏不同采收期总生物碱含量以 8月中下旬最高 ,每株平均总生物碱产量以 1 0月中下旬至 1 1月上旬最高 ,半夏最佳采收期以 1 0月中下旬至 1 1月上旬为宜     

Exploring the relationship between reflectance red edge and chlorophyll concentration in slash pine leaves

Chlorophyll concentration is related positively to the point of maximum slope in the reflectance spectra of leaves and this point is termed the red edge. The reflectance spectra of slash pine (Pinus elliottii Engelm.) needles were measured in the field and the chlorophyll concentrations of the same needles were measured in the laboratory. The measurement errors for red edge and chlorophyll concentration were determined to be 2.2 nm (3% of mean) and 0.35 mg g(-1) (19% of mean), respectively. The red edge-chlorophyll concentration relationship was strong (r(2) = 0.82, n = 152). A red edge-chlorophyll concentration relationship for n = 100 was used with red edge measurements to estimate chlorophyll concentration with an rms error of 0.31 mg g(-1) (17% of mean, n = 52). The entire red edge-chlorophyll concentration relationship for n = 152 was also used with red edge measurements to estimate the chlorophyll concentration of samples from an earlier experiment with an rms error of 0.47 mg g(-1) (30% of mean, n = 38). We conclude that measures of red edge can be used to estimate the chlorophyll concentration of detached needles in the field with an accuracy similar to that obtained by conventional laboratory measurements.     

A method for routine measurements of total sugar and starch content in woody plant tissues

Several extraction and measurement methods currently employed in the determination of total sugar and starch contents in plant tissues were investigated with the view to streamline the process of total sugar and starch determination. Depending on the type and source of tissue, total sugar and starch contents estimated from samples extracted with 80% hot ethanol were significantly greater than from samples extracted with a methanol:chloroform:water solution. The residual ethanol did not interfere with the sugar and starch determination, rendering the removal of ethanol from samples unnecessary. The use of phenol-sulfuric acid with a phenol concentration of 2% provided a relatively simple and reliable colorimetric method to quantify the total soluble-sugar concentration. Performing parallel sugar assays with and without phenol was more useful for accounting for the interfering effects of other substances present in plant tissue than using chloroform. For starch determination, an enzyme mixture of 1000 U alpha-amylase and 5 U amyloglucosidase digested starch in plant tissue samples more rapidly and completely than previously recommended enzyme doses. Dilute sulfuric acid (0.005 N) was less suitable for starch digestion than enzymatic hydrolysis because the acid also broke down structural carbohydrates, resulting in overestimates of starch content. After the enzymatic digestion of starch, the glucose hydrolyzate obtained was measured with a peroxidase-glucose oxidase/o-dianisidine reagent; absorbance being read at 525 nm after the addition of sulfuric acid. With the help of this series of studies, we developed a refined and shortened method suitable for the rapid measurement of total sugar and starch contents in woody plant tissues.     

木麻黄枝叶中单宁含量的快速测定

采用皮粉法与胶体滴定法测得pH=7时木麻黄树皮单宁的胶体滴定值与单宁质量的标准曲线,所得标准曲线的线性回归方程为:y=0.4852x+0.8755,线性系数R2=0.9997。再用胶体滴定法滴定来自同一株木麻黄树的叶、粗枝和细枝的浸提液,根据胶体滴定值在标准曲线上对应的单宁质量计算出干体各部位的单宁含量。木麻黄的叶、粗枝和细枝的单宁含量分别为12.11%、7.31%和6.29%,相对极差R小于2%。     

石墨炉原子吸收标准加入校正法测定土壤中痕量镉

选用硝酸-氢氟酸-高氯酸、硝酸-盐酸-氢氟酸-高氯酸2种消解体系,建立了石墨炉原子吸收标准加入校正法测定土壤中镉的方法,能够实现对土壤镉的准确测定.以硝酸钯为基体改进剂,优化灰化温度为550℃,原子化温度为1600℃.分别取土壤标准样品GBW07452、GBW07388经微波消解或全自动消解后,定量加入到标准溶液系列中...     

Determination of 2-thiocyanomethylthiobenzothiazole (TCMTB) in treated wood and wood preservative using Ultraviolet–visible spectrophotometer

Ultraviolet–visible Spectrophotometer method for the determination of 2-thiocyanomethylthiobenzothiazole (TCMTB) in treated wood and wood preservative was developed. The determination was done after conversion of TCMTB to 2-mercaptobenzothiazole (2-MBT). This conversion was obtained by reaction with 0.1?M cystein alkaline condition (pH 10). The extraction of 2-MBT was carried out with ethyl acetate containing 0.2% of ?-mercaptoethanol after acidification with 2?M phosphoric acid (pH 2.5). The sample absorbance was measured at 324?nm wavelength with a calibration curve range from 10 to 90?ppm of TCMTB. The Regression value, R ², achieved was 0.9998, while the precision, RSD, was <10% (n?=?6). The recovery was in the range of 90.7–103.2% (n?=?6). The result obtained with this colorimetric procedure is comparable to the HPLC–PDA method.     

Variability in permeability and integrity of cell membrane and depletion of food reserves in neem （Azadirachta indica） seeds from trees of different age classes

We quantified cell membrane permeability(electrical conductivityEC,water soluble sugar-WSS,and amino acids-AA)and integrity(phospholipids,α-tocopherol and lipid peroxidation)along with food reserve deterioration(total proteins,total sugar,and total starch)of neem seeds collected from various mother tree age classes and stored for 65days in airtight plastic containers at ambient room temperature(35±5°C).Results show that the activities were higher in fresh seeds(EC267.56-2950.01μS/g,WSS 19.96-19.48 mg/g and AA 5.40-5.35 mg/g)and declined with increasing duration of storage period(EC153.37-195.17μS/g,WSS 3.13-4.17 mg/g and AA 4.29-4.49 mg/g after35 days and EC 144.02-161.56μS/g,WSS 2.06-2.40 mg/g and AA3.98-4.27 mg/g after 65 days of storage).Phospholipids andα-tocopherol were higher in fresh seed(0.073-0.093 OD at 710 nm and0.080-0.105 OD,respectively)and declined as storage duration increased(0.033-0.042 OD at 710 nm and 00.0010-0.0020 OD,respectively).Dead seeds showed reduced amounts of phospholipids and minimum activity ofα-tocopherol(antioxidants).The level of MDA was lower in fresh seeds(0.0066-0.0087 OD at 600-535 nm)and increased as storage duration increased(0.0248-0.0268 OD after 65 days of storage).The higher amount of MDA indicated that seeds died due to rancidity of the oil inside the seed.Neem seed cake was assessed for deterioration of food reserves(total proteins,total sugar,and total starch),concentrations of which were higher in fresh seed and declined as storage duration increased.Germination was higher in fresh seeds and after 65days,no germination was received perhaps due to deterioration of biochemicals in seeds.Patterns of seed deterioration were similar across all seed lots.