RP-HPLC法测定落叶松中二氢槲皮素的含量

采用反相高效液相色谱法测定落叶松中二氢槲皮素的含量。确定色谱条件为：色谱柱Hypersil ODS—C18（4．6mm×200mm,5μm）;流动相为V（甲酵）：V（水）：V（冰醋酸）=40：59：1;流速为1．0mL·min^-1;检测波长为288nm;柱温为28℃。在此条件下,二氢槲皮素与其它组分得到良好的分离。线性范围为0．02～0．2μg·μL^-1（r=0．9998）,精密度RSD为0．96％（n=5）,平均回收率为100．4％。     

水杨菌胺高效液相色谱分析方法

采用反相高效液相色谱法，以甲 水＝85＋15（v/v)(pH=4.2)为流动相，用紫外检测器对水杨菌胺进行分离和测定。结果表明：水杨菌胺含量测定的精密标准偏差为0．34，变异系数为0．39％，回收率为98．5－100．1％，线性相关系数为0．996。     

HPLC法测定粉萆薜和绵萆薜中薯蓣皂苷元的含量

建立了高效液相色谱法对粉革薜和绵萆薜药材中薯蓣皂苷元的含量测定方法,通过测定比较两者含量大小。方法：采用反相高效液相色谱法：色谱柱为Gemini C18（250mm×4．6mm,5μm）,甲醇：水（95：5）为流动相,流速：1．0ml Mmin,检测波长：210nm,对粉、绵萆薜药材中的薯蓣皂苷元进行含量测定。结果表明：线性范围为0．1205—1．205mg／mL,r=0．9997,平均回收率99．59％,RSD=0．46％（n=5）,粉革薜的平均含量为0．4811mg／mL,绵革薜的平均含量为0．1010mg／mL。本实验方法简便,快速,结果可靠,可用于对粉、绵萆薜药材中薯蓣皂苷元的含量测定,得出粉革薜中薯蓣皂苷元的含量远大于绵革薜中的含量。     

高效液相色谱法测定三（3-羟丙基）膦溶液中催化剂V601的含量

建立了高效液相色谱法测定三（3-羟丙基）膦反应液中催化剂V601的方法,采用Shim—PackVp—ODS050mm×4．6mm）色谱柱。紫外检测器。在优化的条件下,外标法进行定量分析。结果,用高效液相色谱法测定三（3-羟丙基）膦反应液中催化剂V601的最佳条件为：Shim—packVp—ODS（150mm×4．6mm）色谱柱,流动相为乙腈／水（v／v=8：2）,紫外检测波长为200nm,流速为1．0mL·min-1。结论：该方法具有简便、快速、准确、灵敏度高、重现性好的特点。     

HPLC法测定注射用盐酸氨溴索中的含量及有关物质

采用Diamonsil C18柱（200mm×4．6mm,5μm）,以0．1mol／L磷酸二氢钾（pH值7．04-0．05）-乙腈（40：60）为流动相,流速为1．0mL·min^-1,检测波长为248nm,柱温：室温。建立高效液相色谱法测定注射用盐酸氨溴索中盐酸氨溴索的含量及有关物质。盐酸氨溴索的线性范围为20-100 μg·mL^-1,相关系数r=0．9997;平均回收率为99．90％（n=9）。该方法简便、准确、专属,可用于注射用盐酸氨溴索的含量及有关物质的测定。     

柱前衍生反相高效液相色谱法快速测定3,5-二氯苯甲酰氯

以无水甲醇作柱前衍生试剂，建立了反相高效液相色谱法间接测定3，5-二氯苯甲酰氯的新方法。实验结果表明，在流动相：甲醇-水（85：15），流速：1．0mL／min，检测波长：288nm的条件下，定量校正曲线具有良好的线性关系，相关系数（r）为0．9999。方法用于样品中标题物质的测定，RSD=0．19％（n=6），加标回收率为99．9％-105％。     

4，4′-二（羟甲基）联苯合成回收溶剂中二甲亚砜含量的测定方法

采用高效液相色谱法测定4,4′-二（羟甲基）联苯合成后回收溶剂中二甲亚砜的含量。方法采用Zorbax SB-C18色谱柱,以甲醇-水（v：v=13：7）为流动相,检测波长为210nm,标准曲线外标法测定回收溶剂中二甲亚砜的含量。二甲亚砜在0．08-0．58mg／mL浓度范围内与峰面积呈线性关系,回归方程：y=14．8594x＋154．7371,相关系数r=0．99996。平均回收率为100．59％,RSD为0．69％（n=6）。     

硫磷酯高效液相色谱分析

采用Kromasil C18反相柱为色谱柱,乙睛：水=65：35（v／v）为流动相,紫外检测器在210nm对农药乐果中间体-硫磷酯进行高效液相色谱分离和测定。其线性相关系数为0．9999,变异系数为0．1％,回收率为99．4％～100．4％。     

烟嘧·莠去津油悬浮剂的高效液相色谱分析

采用高效液相色谱法,以Hypersil C18（250×4．6mm,10μm）为固定相,以乙腈＋甲醇＋水＋冰醋酸=300＋200＋500＋5（v＋y）为流动相,流速1．0mL·min^-1,检测波长254nm,在同一色谱条件下同时测定烟嘧·莠去津油悬浮剂中的烟嘧磺隆和莠去津。烟嘧磺隆变异系数为2．21％,平均回收率为100．4％,莠去津变异系数为0．77％,平均回收率为99．5％。     

HPLC法测定妇科止血灵胶囊芍药苷的含量

建立妇科止血灵胶囊高效液相色谱法测定芍药苷的方法。色谱柱：DiamonsilCl8（4．6mm×250mm,5μm）。流动相：乙腈-0．1％磷酸溶液（14：86）。流速：1．0mL·min-1。检测波长：230nm。柱温：35℃。进样量：10μg。芍药苷在12．6-252．0μg／mL范围内呈良好线性关系,r=0．9997。平均加样回收率为98．37％,RSD=1．34％（n=5）。所建立的方法简便准确、灵敏度高,可作为妇科止血灵胶囊的质量控制方法。     

Optimization of Microwave-Assisted Extraction of Tea Saponin and Its Application on Cleaning of Historic Silks

Microwave-assisted extraction (MAE) was utilized to extract tea saponin from oil-tea camellia seed cake. The factors influencing the extraction efficiency were studied, including the effects of microwave power, irradiation duration, temperature, ratio of solvent to material and aqueous ethanol concentration. By systematic orthogonal experiments, the optimal extraction technology was determined. Compared with a conventional extraction method, MAE shows great advantages with the extraction time reduced from 6 h to 4 min, 50 % organic solvent saved and about 14 % extraction yield enhanced. Fourier transform infrared spectroscopy testing and high performance liquid chromatography analysis proved that the extracted resultants were tea saponin with similar compounds as a standard tea saponin. The extracted tea saponin was applied on the cleaning of historic silks and showed good removal effect on the stains. This work provides useful information for fully use of oil-tea camellia seed cake and new applications of tea saponin at the protection of historic textiles.     

Über das türkische Teesamenöl und Teesaponin

Turkish Teaseed Oil and Tea Saponin The annual production of black tea in Turkey is about 50 000 t. It is estimated, that Turkey can produce annually 14 000 t tea seed and 3000 t teaseed oil. The seed consists of 70% kernel and 30% hull. The oil content of the kernel is 33%. The Turkish teaseed oil has following characteristics: Specific weight at 25° C: 0.9180; refractive index at 25° C: 1.4692; saponification value: 192.8; iodine value (Hanus): 90.9; RM-value: 1.0; hydroxyl value: 5.25; unsaponifiable: 1.05%. Gas chromatographic determination of fatty acids gave following average values: myristic acid traces, palmitic acid 16.0%, stearic acid 1.67%, oleic acid 59.4%, linoleic acid 21.8% and arachidic acid 1.23%. The oilcake contains 14% saponin, therefore, has a bitter taste. Tea saponin is a triterpenic saponin of the type of amyrin. The aglycone consists of five different sapogenins. The carbohydrate part of the tea saponin contains following sugars: xylose, galactose, glucose and galacturonic acid.     

茶皂素提取条件的优化及纯化研究

以油茶茶籽粕为原料，采用乙醇水溶液提取茶皂素。在茶籽粉和乙醇料液比1 : 9(g : mL)，乙醇体积分数60%，提取温度60 ℃和提取时间3 h的最佳条件下茶皂素的提取得率达14.9%。用NKA-9型大孔吸附树脂吸附纯化茶皂素粗品，树脂静态吸附与解吸结果表明：树脂静态吸附茶皂素粗提液0.5 h基本饱和，体积分数80%乙醇解吸率为91.1%；动态吸附与解吸时，上样流速8 mL/min较佳，吸附率为66.04%，体积分数80%乙醇洗脱，洗脱流速5.0 mL/min，洗脱体积50 mL时，可使流出液中茶皂素质量浓度在1.25~1.57 g/L之间，茶皂素纯度为95%。     

大孔树脂对茶皂素的动态吸附工艺优化

以60％的粗茶皂素为原料,考察了不同大孔树脂对茶皂素的纯化效果,确定用A型树脂进行纯化。研究得出较佳动态吸附一脱附优化工艺为：乙醇浓度50％、上样液浓度30mg／mL、上样液流速1BV／h：洗脱液浓度80％、洗脱剂用量1．75BV、洗脱液流速为1BV／h。在此条件下树脂对茶皂紊的吸附率为96．07％,洗脱率达90．23％,所得茶皂素的纯度达88.90％。     

Separation of Tea Saponin by Two-Stage Continuous Foam Fractionation

A technology of two-stage continuous foam fractionation for tea saponin recovery was studied for increasing both the enrichment ratio and the recovery percentage. In the first stage, the effect of air flow rate, the initial pH, the feed flow rate, and the feed position were studied at a temperature of 60°C. The results showed that when the conditions of the first stage were at a temperature of 60°C, air flow rate 150 mL/min, pH 5.3, feed flow rate 1.92 mL/min, and feed position at the interface between the liquid phase and the foam phase, the enrichment ratio, and the recovery percentage of tea saponin were 4.02 and 56.4%, respectively, and the effluent solution was added to the second stage as the initial solution. When the conditions of the second stage were at a temperature of 30°C and an air flow rate of 300 mL/min, the recovery percentage of tea saponin reached 47.6%, and the foamate was added to the first stage as feed solution. The total recovery percentage of tea saponin reached 86.3% by the two-stage continuous foam fractionation.     

乙醛酸和草酸的高效液相色谱分析

采用高效液相色谱法测定了草酸电合成乙醛酸中乙醛酸和草酸的含量,方法简便,成本低廉,效果良好。色谱柱为VP-ODS(150 mm×4.6 mm),流动相为稀磷酸水溶液(pH=2.7),流速为0.5 mL/min,柱温40℃,检测波长为212 nm。探讨了pH值及其它条件对色谱分离的影响。乙醛酸的线性方程为:Y=1.226×102X-7.053×102,线性相关系数R=0.999 6,相对标准偏差为1.5%,检出限为3.0×10-9g;草酸的线性方程为:Y=1.670×103X-5.563×104,线性相关系数R=0.999 9,相对标准偏差为0.8%,检出限为2.3×10-10g。     

从茶籽饼粕中提取茶皂素的研究

叙述了大孔吸附树脂法提取茶皂素工艺。结果表明 ,取等量茶皂素提取液 12 0mL ,大孔树脂法得茶皂素产量 10 98g ,茶皂素质量分数 91 7% ,正丁醇萃取法产量 5 86g ,茶皂素质量分数78.0 %     

Production of Saponin Biosurfactant from <Emphasis Type="Italic">Glycyrrhiza glabra</Emphasis> as an Agent for Upgrading Heavy Crude Oil

Saponins are the main group of phytogenic biosurfactants extracted from plants. One of the significant applications of these compounds is upgrading and viscosity reduction of heavy crude oil water in oil (W/O) emulsions. In this research, use of saponin extracted from Glycyrrhiza glabra was investigated for viscosity reduction of heavy crude oil and upgrading its API properties. The extracted saponin was characterized using Fourier transform infrared (FTIR) and nuclear magnetic resonance (NMR) spectroscopy. Phase behavior analysis demonstrated a reduction in initial viscosity and improved API gravity of the heavy oil from 2350 mPa·s and 19 to 900 mPa·s and 27, respectively. In addition, the emulsification index (E ₂₄) was found to be 98 % at a saponin concentration of 8 % w/v. It was observed that the emulsions were stable in the pH range of 5.5–13, temperature from 30 to 80 °C and salinity up to 6 % w/v of NaCl solution. Average diameter of W/O droplets evaluated by dynamic light scattering (DLS) were in the range of 10–15 µm. The results obtained from the present research revealed that the extracted saponin improved the physical characteristics of heavy crude oil. We propose the use of saponin as a potential alternative to conventional emulsifiers for upgrading heavy crude oil in petroleum industry.     

茶皂甙纯化工艺研究

对茶皂甙的提取纯化工艺进行了研究。以含量为70%的粗茶皂甙为原料,经N,N-二甲基甲酰胺溶解、乙酸乙酯沉析、胆甾醇复合吸附、苯解吸工艺得到含量大于99%的茶皂甙,提取率大于80%。结果表明,该工艺为高纯度茶皂甙的制备提供了参考。     

乙醇提取-丙酮沉淀法提取分离茶皂素的工艺研究

以油茶饼粕为原料,采用乙醇提取-丙酮沉淀法对茶皂素进行提取分离。以茶皂素纯度和得率为考察指标,对乙醇体积分数、液料比、提取温度、提取时间、提取次数、提取液浓缩程度和丙酮用量等工艺参数进行了单因素优化。结果表明：体积分数95%的乙醇为提取溶剂,乙醇与预处理过的油茶饼粕液料比为9：1（mL：g）,提取温度为70℃,提取时间为4 h,提取次数为2次,提取液浓缩至刚好有固体析出,丙酮用量为4倍浓缩液体积量时提取分离效果较佳,得到的茶皂素纯度为85.17%,得率为9.82%。不同溶剂打浆对产品纯化效果的比较发现：丙酮、乙酸乙酯、无水乙醇、体积分数95%的乙醇作为打浆纯化溶剂用于提高茶皂素纯度效果均不明显。