Simultaneous determination of 12, 13-dihydroxyeuparin and glycyrrhizic acid in Yanyanfang mixture by high performance liquid chromatography

A reversed phase high performance liquid chromatography （HPLC） method was established for the simultaneous determination of 12, 13-dihydroxyeuparin and glycyrrhizic acid in Yanyanfang mixture. A Grace Apollo Cl8 column （250 mm × 4.6 mm, 5 μm） was used as the stationary phase and the mobile phase was composed of acetonitrile and aqueous phosphoric acid （0.2%, v/v）. Gradient elution was carried out at the flow rate of 1.0 mL/min and the column temperature was 30 ℃. An ultraviolet （UV） detector was used with a selected wavelength of 240 nm. Calibration curves were linear within the concentration range of 4.6-45.75 μg/mL for 12, 13-dihydroxyeuparin （r〉0.9999） and 106.9-1068.9μg/mL for glycyrrhizic acid （r〉0.9999）, respectively. Recoveries were 102.18% for 12, 13-dihydroxyeuparin and 101.17% for glycyrrhizic acid. The method developed could be applied to the simultaneous determination of 12, 13- dihydroxyeuparin and glycyrrhizic acid in Yanyanfang mixture.     

Identification and determination of the major constituents in traditional Chinese medicine Longdan Xiegan Pill by HPLC-D

A novel and sensitive HPLC-UV method has been developed for the simultaneous determination of twelve major compounds in Longdan Xiegan Pill.The chemical profile of the twelve compounds,including geniposidic acid（1）,geniposide（2）,gentiopicroside（3）,liquiri     

Simultaneous determination of captopril and hydrochlorothiazide by time-resolved chemiluminescence with artificial neura

The combined use of chemometrics and chemiluminescence（CL）measurements,with the aid of the stopped-flow mixing technique,developed a simple time-resolved CL method for the simultaneous determination of captopril（CPL）and hydrochlorothiazide（HCT）.The stoppe     

Rapid determination of volatile constituents in safflower from Xinjiang and Henan by ultrasonic-assisted solvent extraction and GC-MS

The total volatile components were extracted from safflower by ultrasonic-assisted solvent extraction （USE） and their chemical constituents were analyzed by gas chromatographymass spectrometry （GC-MS） to provide scientific basis for the quality control of safflower. Five different solvents （diethyl ether, ethanol, ethyl acetate, dichloromethane and acetone） were used and compared in terms of number of volatile components extracted and the peak areas of these components in TIC. The results showed that USE could be used as an efficient and rapid method for extracting the volatile components from safflower. It also could be found that the number of components in the TIC of ethyl acetate extract was more than that in the TIC of other solvent ones. Meanwhile, the volatile components of safflower from Xinjiang Autonomous Region and Henan Province of China were different in chemical components and relative contents. It could be concluded that both the extraction solvents and geographical origin of safflower are responsible for these differences. The experimental results also indicated that USE/GC-MS is a simple, rapid and effective method to analyze the volatile oil components of safflower.     

局域电荷体系的电势

探讨了分布在小区域v内的连续电荷体系在远场所产生的电势，可表为一组位于原点的各级多极子在远场产生的电势的叠加，而连续分布电荷体系可用位于原点的各级多极子代替．     

Chemiluminescence determination of melamine with Luminol-K3Fe（CN）6 system

A sensitive chemiluminescence（CL） method was developed for determining melamine in urine and plasma samples based on the fact that melamine can remarkably enhance the chemiluminescence of Luminol-K3 Fe（CN）6 system in alkaline medium. The determination con     

Quantification of six bioactive compounds in Zhenqi Fuzheng preparation by high-performance liquid chromatography couple

A simple and accurate high-performance liquid chromatography（HPLC）coupled with diode array detector（DAD）and evaporative light scattering detector（ELSD）was established for the determination of six bioactive compounds in Zhenqi Fuzheng preparation（ZFP）.The     

乳化沥青冷再生试验方法改进及性能研究

对《公路沥青路面再生技术规范》（JTG F41-2008）中乳化沥青冷再生混合料试验规程中的最佳含水率OWC的确定方法以及试件成型的养生温度等进行改进,以完善和简化规范要求的试验方法,并通过室内试验对改进后的试验方法进行验证和对比研究。研究表明,使用最佳流体含量OFC作为乳化冷再生混合料外加水的控制指标优于规范要求的最佳含水量OWC指标;提高试验养生温度至110℃,可以获得与规范60℃养生温度相似的结果,并能够缩短试验所需时间,提高工作效率;乳化沥青冷再生混合料具有较好的水稳定性能及高温稳定性能,能满足或高于热拌沥青混合料的技术要求。     

LC-MS determination and pharmacokinetic study of salidroside in rat plasma after oral administration of suspensions of t

A simple,rapid and sensitive liquid chromatography-mass spectrometry（LC-MS）method was developed for the determination of salidroside in rat plasma and study of its pharmacokinetics after oral administration of suspension of Erzhi Wan and Fructus Ligustri     

Flow injection chemiluminescence determination of loxoprofen and naproxen with the acidic permanganate-sulfite system

A novel flow injection chemiluminescence（CL）method for the determination of loxoprofen and naproxen was proposed based on the CL system of KMnO4 and Na2SO3 in acid media.The CL intensity of KMnO4-Na2SO3 was greatly enhanced in the presence of loxoprofen a     

Rapid europium-sensitized fluorescent determination of ulifloxacin,the active metabolite of prulifloxacin,in human serum

A new fluorescent method was developed based on the ulifloxacin-europium（Ⅲ）-sodium dodecylbenzene sulfonate system for the determination of ulifloxacin,the active metabolite of prulifloxacin.Sodium dodecylbenzene sulfonate formed a ternary complex with ul     

Analysis and determination of diterpenoids in unprocessed and processed Euphorbia lathyris seeds by HPLC-ESI-MS

Euphorbia lathyris （Caper spurge） is a toxic and potent Chinese materia medica （T/PCMM）. This study sought a method for identifying five diterpenoids （Euphorbia factors LI-L3, L7a, and Ls） with the spectra of UV and mass, quantifying three diterpenoids L1, L2, and L8 in crude extracts of unprocessed and processed E. lathyris seeds by liquid chromatography/ electrospray ionization mass spectrometry （LC-ESI-MS）. The analysis was achieved on an Agilent Eclipse XDB-C18 column （4.6 mm× 150mm i.d., 5 μm） with an isocratic elution with a mobile phase consisting of water and acetonitrile at a flow rate of 0.25 mL/min at column temperature of 30 ℃ and UV detection was set at 272 nm. An ESI source was used with a positive ionization mode. The calibration curve was linear in the ranges of 9.9-79 μg/mL for Euphorbia factor Lb 3.8-30.5μg/mL for Euphorbia factor L2, and 1.0-20.6 μg/mL for Euphorbia factor LB. The average recoveries （n=6） of three diterpenoids were 98.39%, 91.10% and 96.94%, respectively, with RSD of 2.5%, 2.4% and 2.1%, respectively. The contents of the three diterpenoids in processed E. lathyris seeds were 3.435, 1.367 and 0.286 mg/g, respectively, which decreased more sharply than those in unprocessed E. lathyris seeds which were 4.915, 1.944 and 0.425 mg/g, respectively. The method is simple, accurate, reliable and reproducible, and it can be applied to control the quality of unprocessed and processed E. lathyris seeds.     

高效液相色谱法测定水溶液中芘的实验研究

建立表面活性剂与有机物共存体系中芘测定的高效液相色谱法.采用C18反向色谱柱(2.1mm×100mm,5μm),通过调节和控制流动相、柱温、流速等因素,得到芘的优化测试条件.结果表明:流动相选用乙腈-水(80:20,V/V),流速0.20mL·min-1,柱温25℃是最优测试条件.同时,对TX-100存在与不存在情况下芘的测试结果进行比较分析,使用OriginPro 8.6对实验数据进行线性拟合,并进行统计学t检验,结果表明:X-100存在与否对水溶液中芘的测定没有显著影响.     

用回弹法推定"标号混凝土强度"的方法

针对现行《回弹法检测混凝土抗压强度技术规程》（JGJ/T23—2001）中的混凝土强度推定方法,对设计标号和强度等级验收水平及其关系进行分析,建议用回弹法推定混凝土强度时应考虑被测构件的设计标准和施工控制标准,以尽量符合原设计、施工水平,做出客观的评价。     

一种新型道路缓和曲线的线形分析与评价

缓和曲线作为一种空间过渡曲线,其设计的合理与否直接关系到车辆行驶的平稳性和旅客舒适性。介绍了利用缓和曲线边界条件确定其代数方程式的一种通用方法：根据边界条件列出曲率待定方程,并利用曲率边界条件确定出缓和曲线曲率方程,然后对曲率方程二次积分得到缓和曲线的方程。此方法适用于推导缓和曲线方程,可为公路缓和曲线线形设计提供参考。采用此方法设计出了一种连接直线与直线的新型缓和曲线,并建立5种不同工况,以横向加速度及其时变率为评价指标,对新型缓和曲线和回旋线进行了行驶动力学性能评价,通过比较分析得出这种新型缓和曲线在行驶动力学性能上明显优于回旋线,为高速公路缓和曲线的线形选择提供参考。     

Analysis of chiral non-steroidal anti-inflammatory drugs flurbiprofen, ketoprofen and etodolac binding with HSA

The protein binding of non-steroidal anti-inflammatory drugs flurbiprofen, ketoprofen and etodolac with human serum albumin （HSA） was investigated using indirect chiral high performance liquid chromatography （HPLC） and ultrafiltration techniques. S-（-）-1-（1-naphthyl）- ethylamine （S-NEA） was utilized as chiral derivatization reagent and pre-column derivatization RP-HPLC method was established for the separation and assay of the three pairs of enantiomer. The method had good linear relationship over the investigated concentration range without interference. The average extraction efficiency was higher than 85% in different systems, and the intra-day and inter-day precisions were less than 15%. In serum albumin, the protein binding of etodolac enantiomers showed significant stereoselectivity that the affinity of S-enantiomer was stronger than R-enantiomer, and the stereoselectivity ratio reached 6.06; Flurbiprofen had only weak stereoselectivity in HSA, and ketoprofen had no stereoselectivity at all. Scatchard curves showed that all the three chiral drugs had two types of binding sites in HSA.     

Chemiluminescence enzyme immunoassay based on magnetic nanoparticles for detection of hepatoceUular carcinoma marker glypican-3

Glypican-3 （GPC3） is reported as a great promising tumor marker for hepatocellular carcinoma （HCC） diagnosis. Highly sensitive and accurate analysis of serum GPC3 （sGPC3）, in combination with or instead of traditional HCC marker alpha-fetoprotein （AFP）, is essential for early diagnosis of I-ICC. Biomaterial-functionalized magnetic particles have been utilized as solid supports with good biological compatibility for sensitive immunoassay. Here, the magnetic nanoparticles （MnPs） and magnetic microparticles （MmPs） with carboxyl groups were further modified with streptavidin, and applied for the development of chemiluminescence enzyme immunoassay （CLEIA）. After comparing between MnPs- and MmPs-based CLEIA, MnPs-based CLEIA was proved to be a better method with less assay time, greater sensitivity, better linearity and longer chemiluminescence platform. MnPs-based CLEIA was applied for detection of sGPC3 in normal liver, hepatocirrhosis, secondary liver cancer and HCC serum samples. The results indicated that sGPC3 was effective in diagnosis of HCC with high performance.     

Quantitative analysis of a novel antimicrobial peptide in rat plasma by ultra performance liquid chromatography-tandem mass spectrometry

We described the first results of a quantitative ultra performance liquid chromatographytandem mass spectrometry method for a novel antimicrobial peptide （phylloseptin, PSN-1）. Chromatographic separation was accomplished on a Waters bridged ethyl hybrid （BEH） C18 （50mm× 2.1 mm, 1.7 μm） column with acetonitrile-water （25：75, v/v） as isocratic mobile phase. Mass spectrometry detection was performed in the positive electrospray ionization mode and by monitoring of the transitions at m/z 679.6/120, 509.6/120 （PSN-1） and m/z 340.7/165 （Thymopentin, IS）. Protein precipitation was investigated and the recovery was satisfactory （above 82%）. The method was shown to be reproducible and reliable with intra-day precision below 5.3%, inter-day precision below 14.2%, and linear range from 0.02 to 2 lag/mL with r〉0.994. The method was successfully applied to a pharmacokinetic study of PSN-1 in rats after intravenous administration.     

The clinical value of enzyme-multiplied immunoassay technique monitoring the plasma concentrations of cyclosporine A a

The feasibility and the clinical value of the enzyme-multiplied immunoassay technique （EMIT） monitoring of blood concentrations of cyclosporine A （CsA） in patients treated with CsA were investigated after kidney transplantation. The validation method was     

AS-X树脂的增韧及耐候性研究

用马来酸酐MAH熔融接枝POE制得POE-g-MAH,用其作为AS与POE的相容剂,提高AS树脂韧性与耐候性,并研究了PE-g-MAH和PP-g-MAH作为相容剂PC/AS共混物的增韧作用.用摆锤式冲击试验机、拉伸试验机测试增韧效果,用SEM,FTIR,DSC等测试手段研究产物及共混物的共组成、相容性、相结构、热稳定性.结果表明：PC/AS共混物增韧效果比POE-g-MAH/AS好,PC/AS共混物缺口冲击强度达到5.45 J/m2几乎是纯AS树脂（1.2 kJ/m2）的5倍.