高效液相色谱法测定天女木兰叶中游离酚和结合酚

[目的]进一步了解天女木兰中酚类物质种类及含量。[方法]利用高效液相色谱仪对天女木兰叶片中游离酚、结合酚和酯化酚进行定性定量测定。[结果]在10种检测酚中,天女木兰叶片中含有香豆酸和绿原酸2种游离酚,含有咖啡酸、香豆酸、香豆素和表儿茶素4种结合酚及香豆素和香豆酸2种酯化酚;各种形式的香豆酸广泛存在于叶片中。[结论]该研究建立的高效液相色谱法测定天女木兰叶中游离酚和结合酚的方法准确、可靠。     

HPLC法测定玉米酒糟中绿原酸的含量

采用浸提法提取玉米酒糟中绿原酸并用HPLC法测定其中的含量,采用安捷伦色C18（4.6mm×150mm,5μm）色谱柱,乙腈-0.5％磷酸溶液为流动相,流速为1.0mL·min-1,检测波长为327nm.结果表明绿原酸在0.232～2.784μg呈现良好的线性关系,玉米酒糟中绿原酸含量0.028％,平均回收率为95.80％,RSD=2.72％.试验证明了玉米酒糟中含有绿原酸,且其含量较高,为玉米酒糟的进一步开发提供科学依据.     

Evaluation of Commercial Fe(III)‐Chelates Using Different Methods

Abstract

A collaborative assay among three laboratories was made in order to compare both the ion (CEN. EN 13368‐2:2001 E. Determination of chelating agents in fertilizers by ion chromatography. Part 2: EDDHA and EDDHMA, 2001a) and the ion‐pair (Lucena, J.J.; Barak, P.; Hernandez‐Apaolaza, L. Isocratic ion‐pair high‐performance liquid chromatographic method for the determination of various iron(III) chelates. J. Chromatogr. A 1996, 727, 253–264) high performance liquid chromatography (HPLC) methods as well as the soluble and complexed Fe (CEN. EN 13366:2001 E. Treatment with a cation exchange resin for the determination of the chelated micronutrient content and of the chelated fraction of micronutrients, 2001b) methods. Fifteen and ten samples of commercial fertilizers of Fe‐EDDHA, Fe‐EDDHMA, respectively were analysed by three laboratories using these methods. No significant differences were observed between the results obtained for the Fe‐EDDHA content using the Lucena et al. or CEN method. The first method makes it possible to distinguish between the meso and DL‐racemic diasteroisomers of Fe‐o, o‐EDDHA. For the Fe‐EDDHMA formulations, the CEN method gives higher values than the ion‐pair method, since in the first one Fe‐EDDH4,6MA coelutes with FeEDDHMA. Also the CEN method does not makes it possible to distinguish between Fe‐EDDHMA and Fe‐EDDH5MA products. The variability among laboratories was larger for the CEN method than for the Lucena et al. method.     

黄连及黄连须、黄连茎叶体外抗氧化活性的谱效关系研究

测定黄连与黄连须、黄连茎叶主要生物碱含量并建立高效液相(HPLC)指纹图谱,分析其抗氧化活性的谱效关系。采用HPLC分析比较黄连及黄连须、黄连茎叶中小檗碱、表小檗碱、药根碱、黄连碱、巴马汀含量差异并建立指纹图谱,通过羟自由基(·OH)、1,1-二苯基-2-三硝基苯肼(DPPH)自由基、2,2-联氮基双(3-乙基苯并噻唑啉-6-磺酸)(ABTS)自由基体外清除试验与总还原力试验评价其体外抗氧化活性差异,应用Pearson相关系数法分析HPLC指纹图谱与抗氧化活性的谱效关系。结果发现小檗碱、巴马汀含量为黄连>黄连茎叶>黄连须;药根碱、黄连碱和表小檗碱含量为黄连>黄连须>黄连茎叶;总还原力为黄连>黄连茎叶>黄连须,·OH、DPPH、ABTS·+自由基清除力为黄连茎叶>黄连>黄连须;总还原力与各峰均有较强相关性,·OH、DPPH、ABTS·+自由基清除力与4号峰相关性较强。说明黄连茎叶体外抗氧化活性较强,黄连须与黄连茎叶均有一定药用开发价值。     

HPLC法测定天然植物粗提物中芍药苷含量

建立高效液相色谱法检测天然植物粗提物饲料原料中芍药苷的测定方法。用十八烷基硅烷键合硅胶色谱柱,以乙腈-0.1%磷酸溶液(14:86)为流动相,检测波长230nm,流速：1.0 mL/min;柱温：30 ℃;进样量：10μL。结果显示,芍药苷的线性方程为Y=10.6017X－14.8514,(r=0.99966,n=6),本方法的回收率为100.4~102.1%,RSD均小于2.0%。结果表明,本方法准确,可靠,适用于天然植物粗提物饲料原料中芍药苷的测定。     

Residue Detection of Tetracyclines in Eggs by High Performance Liquid Chromatography

The study was aimed to establish the method of simultaneous detection of four kinds of tetracyclines,including oxytraoycline,tetracycline,chlortetracycline and doxyeycline in eggs by high performance liquid chromatography (HPLC).The eggs samples were detected with HPLC after through the procedure of extraction of 0.1 mol/L Na₂EDTA-Mcllvaine buffered solution,purification of Oasis MAX solid-phase extraction column,gradient elution of taking acetonitrile-0.01 mol/mL trifluoroacetic acid as mobile phase,separation with reverse liquid chromatography.The results showed that the calibration curves of four kinds of tetracyclines were linear correlated in the concentration range of 30 to 1 000 ng/g which the limits of detection was 10 ng/g and the limit of quantification was 50 ng/g.The average recoveries were 67.3% to 81.4%,relative standard deviations of intraday was 2.7% to 14.3%,relative standard deviations of inter-day was 0.9% to 5.0%.This mothod established in this study could simultaneously detect oxytetracycline,tetracycline,chlortetracycline and doxycycline drug residues in egg and it had high sensitivity,accuracy and precision.The method was rapid and simple to operate.     

HPLC测定宫衣净酊中葛根素含量

为了建立宫衣净酊中葛根素的高效液相色谱(HPLC)测定方法,应用色谱柱为安捷伦Eclipse XDB-C18(4.6mm×250mm,5μm),流动相为甲醇-水(25∶75),流速为1mL/min,检测波长为250nm,柱温为30℃。结果表明,在此色谱条件下,葛根素的线性范围为18.25μg/mL~584.00μg/mL(r=0.999 9,n=6),平均回收率为108.83%(RSD=1.03%)。说明本方法简便、准确、重现性好,可以作为宫衣净酊的质量控制方法。     

Comparative pharmacokinetics of marbofloxacin in healthy and Mannheimia haemolytica infected calves

The pharmacokinetics of marbofloxacin were investigated in healthy (n=8) and Mannheimia haemolytica naturally infected (n=8) Simmental ruminant calves following intravenous (i.v.) and intramuscular (i.m.) administration of 2 mg kg(-1) body weight. The concentration of marbofloxacin in plasma was measured using high performance liquid chromatography with ultraviolet detection. Following i.v. administration of the drug, the elimination half-life (t(1/2 beta)) and mean residence time (MRT) were significantly longer in diseased calves (8.2h; 11.13 h) than in healthy ones (4.6 h; 6.1 h), respectively. The value of total body clearance (CL(B)) was larger in healthy calves (3 ml min(-1) kg(-1)) than in diseased ones (1.3 ml min(-1) kg(-1)). After single intramuscular (i.m.) administration of the drug, the elimination half-life, mean residence time (MRT) and maximum plasma concentration (C(max)) were higher in diseased calves (8.0, 12 h, 2.32 microg ml(-1)) than in healthy ones (4.7, 7.4 h, 1.4 microg ml(-1)), respectively. The plasma concentrations and AUC following administration of the drug by both routes were significantly higher in diseased calves than in healthy ones. Protein binding of Marbofloxacin was not significantly different in healthy and diseased calves. The mean value for MIC of marbofloxacin for M. haemolytica was 0.1+/-0.06 microg ml(-1). The C(max)/MIC and AUC(24)/MIC ratios were significantly higher in diseased calves (13.0-64.4 and 125-618 h) than in healthy calves (8-38.33 and 66.34-328 h). The obtained results for surrogate markers of antimicrobial activity (C(max)/MIC, AUC/MIC and T > or = MIC) indicate the excellent pharmacodynamic characteristics of the drug in diseased calves with M. haemolytica, which can be expected to optimize the clinical efficacy and minimize the development of resistance.     

烷基-二醇基硅胶填料的合成及对莠去净类除草剂的在线分离

三步合成了烷基-二醇基硅胶(ADS)色谱材料，首先用γ-缩水甘油醚氧丙基三甲氧基硅烷把功能基团键合到硅胶基体上，再把该环氧化硅胶与硬脂酸反应以制备酯型十八烷基反相填料，最后在20MPa压力下装成色谱预柱(35×4.6mm I.D)。用该预柱通过六通阀后接ODS分析柱(250×4.6mm I.D)，构成中心切割二维HPLC。该系统能对具有一定疏水性的化合物进行在线富集，实现环境及生物复杂样品直接进样分离分析。使用该系统对尿中的莠去净和西玛津残留进行了分离分析，以含有0.1%乙酸的酸性水缓冲液对加标尿液中莠去净类化合物保留在预柱上，干扰分析的大分子被排阻而无保留通过，其它干扰分子保留小而通过，再切换六通阀，以乙腈和0.1%乙酸水溶液进行梯度洗脱，进而在下一级ODS分析柱上进行分离（紫外检测225nm），两种除草剂的分离分析取得了良好的定性定量结果     

比久和多效唑混合物的高效液相色谱分析

在吸光度为210nm、流动相配比为甲醇：乙腈：水＝40：20：40的条件下，多效唑和比久均能得到很好的分离。比久的保留时间约为3．19min，多效唑的保留时间约为11．83min。加标回收率：比久为108．69％，多效唑为90．39％。