香丹注射液中丹酚酸B的HPLC法测定

建立了1种测定香丹注射液中丹酚酸B含量的反相高效液相色谱法;色谱分析柱为Hypersil ODS(4.6mm×250 mm,5μm),流动相为甲醇-乙腈-甲酸-水(体积比27∶9∶1.1∶62.9,含10 mmol/L的四丁基溴化铵),检测波长为285 nm,流速为1.0 mL/min,柱温为31℃时,丹酚酸B得到较好的分离;丹酚酸B进样量在0.264~1.584μg范围内线性良好,r=0.999 8,方法平均回收率为98%,为香丹注射液质量控制提供了分析方法。     

场放大进样-扫集胶束电动色谱法测定金银花中的咖啡酸与绿原酸

以场放大进样-扫集胶束电动色谱法( FASI - sweeping-MEKC)测定了金银花中的咖啡酸、绿原酸.考察了SDS浓度、进样电压、进水时间与进样时间比值、进样时间以及缓冲液组成对分离效果的影响.最佳分离条件为:采用未涂层熔融石英毛细管(50 cm × 50 μm,有效柱长33 cm),缓冲体系为100 mmol...     

固相萃取-高效液相色谱法测定化妆品中苯甲酸和山梨酸

化妆品样品用甲醇提取使苯甲酸及山梨酸溶于溶剂中,经离心分离,取上层清液,通过反相C18固相萃取小柱纯化。取其流出液经过滤和脱气后,用于高效液相色谱法分析。取20μL进样,在Hypersil C18反相色谱柱(柱温30℃)上进行分离,所用流动相为甲醇与0.02 mol.L-1乙酸铵(15+85)混合溶液,流量为0.8 mL.min-1。采用紫外检测,检测波长为221 nm,测得苯甲酸和山梨酸的检出限(3S/N)分别为0.04,0.08 mg.L-1。用5 mg.L-1的苯甲酸和山梨酸标准溶液作精密度试验,测得两者的相对标准偏差(n=7)分别为2.8%及2.5%,向实际样品中加上述两种酸的标准溶液作回收试验,测得回收率在85.0%~106.7%之间。     

Atomic Absorption Determination of Metals in Soils Using Ultrasonic Sample Preparation

It was shown that ultrasonic treatment accelerates sample preparation of soil extracts from chernozem into different solvents by a factor of 6 to 60. These extracts are used for the atomic absorption determination of soluble species of Cd, Co, Cr, Cu, Ni, Pb, and Zn. The optimum ultrasound parameters (frequency, intensity, and treatment time) were found for preparing soil extracts containing analytes in concentrations required in agrochemical procedures. Different extractants used to extract soluble heavy metals from soils of a standard chernozem type in agrochemical procedures using ultrasonic treatment were classified in accordance with the element nature.     

高效液相色谱法同时测定催化反应液中氨基葡萄糖盐酸盐和氨基葡萄糖酸

向制备氨基葡萄糖酸的催化反应液中加入亚硝酸盐试剂,在25℃下衍生反应5 min,所得含有氨基葡萄糖盐酸盐和氨基葡萄糖酸衍生物的溶液用作高效液相色谱分析。选用AminexHPX-87H离子排斥色谱柱为固定相,以5 mmol·L^-1硫酸溶液为流动相进行淋洗,用示差折光检测器进行检测,提出了同时测定氨基葡萄糖盐酸盐和氨基葡萄糖酸的高效液相色谱法。2种化合物的色谱峰面积与其浓度均在50 mmol·L^-1以内呈线性关系,检出限（3S/N）依次为0.014,0.034 mmol·L^-1。方法用于5批催化反应液中氨基葡萄糖盐酸盐和氨基葡萄糖酸的测定,加标回收率依次在99.3%～100%,99.2%～102%之间;测定值的相对标准偏差均小于2.5%。     

A Comparison of Sample Preparation Techniques for the Determination of an Organo-phosphorous Pesticide from Water Using Reverse-Phase HPLC

Abstract

A methylene chloride liquid/liquid extraction and Sep-Pak C₁₈ cartridge adsorption techniques were used to quantify the pesticide, Dursban, in contaminated environmental water samples. Results showed a large disparity between Dursban levels using these two techniques, due primarily to the presence of a large adsorbed fraction of pesticide. A Sample Clarification Kit was used to isolate the particulate fraction, which can subsequently be stripped of its adsorbed pesticide compliment by means of a methanol rinse. Lastly, the filtrate from the Sample Clarification Kit may be trace enriched on a Sep-Pak C₁₈ cartridge to isolate the dissolved fraction of pesticide.     

HPLC法同时测定乳酸菌饮料中2种防腐剂和3种甜味剂

建立了一种高效液相色谱法同时测定乳酸菌饮料中2种防腐剂（苯甲酸、山梨酸）、3种甜味剂（乙酰磺氨酸钾、天门冬酰苯丙氨酸甲酯、糖精钠）的方法。样品经12％乙酸锌溶液和12％亚铁氰化钾溶液处理后,用C18色谱柱分离-以甲醇和0．02mol／L乙酸铵溶液为流动相梯度淋洗,紫外检测波长为230,205nm,可在30min内将5种组分完全分离,测定结果的相对标准偏差为1．1％-4．3％（n=5）,加标回收率为90％-102％。     

柱前衍生-高效液相色谱法测定生物检材中的氟乙酸钠

以α-溴苯乙酮酯为衍生化试剂,合成了α-氟乙酸苯乙酮酯(APFA)化合物,并以其为标准,建立了柱前衍生-高效液相色谱法测定生物检材中氟乙酸钠的方法。样品中的氟乙酸钠经酸化,丙酮-水(体积比4∶1)萃取,与α-溴苯乙酮衍生化后进行HPLC分析。色谱条件为:Hypersil ODS柱,乙腈-水(体积比50∶50)为流动相,紫外检测波长为254 nm。α-氟乙酸苯乙酮酯在1×10-5~1×10-2mol/L的浓度范围内与峰面积呈良好的线性关系,线性相关系数为0.999 4,生物样品空白添加实验的回收率为86%~93%,检出限为6.0μmol/L(S/N=3),相对标准偏差(RSD)小于3%。该方法灵敏度高、重复性好,适用于生物检材中氟乙酸钠的测定。     

HPLC Determination of Valproic Acid in Human Serum Using Ultraviolet Detection

Abstract

A sensitive HPLC method with minimal sample preparation and good reproducibility for the determination of valproic acid in serum is described. Serum samples were precipitated using acetonitrile containing diazepam as the internal standard. Chromatography was performed on a Hewlett Packard model 1090 equipped with an octadecylsilane column and a Beckman model 163 variable wavelength detector. The drug and internal standard were eluted isocratically using a mobile phase consisting of 0.01M sodium phosphate monobasic solution, pH 2.3 and acetonitrile (63:37 v/v) followed by a gradient to flush the column before the next sample injection. The flow rate was 2.5 mL/min, the injection volume was 25 μL and the effluent was monitored at 210 nm. The serum standard curve was linear from 2.5-200.0 μg/mL with a correlation coefficient of 0.9994. Day-to-day precision for quality control samples (10.0, 25.0, 75.0 μg/mL serum) ranged from 5.6-9.6% CV. Possible interferences from other drugs which might be administered concurrently were studied. The method has been applied to the analysis of human serum samples.     

Preparation and Characterization of Peroxo Titanic Acid Solution Using TiCl3

The peroxo titanic acid solution was successfully prepared using titanium trichloride as a precursor. The basic properties of the TiO₂ film prepared by the solution were investigated in view of phase change, bandgap energy, crystalline size etc. The film displayed amorphous TiO₂ at room temperature, anatase above 281°C and a mixture of anatase and rutile at 990°C. The crystalline size increases with annealing temperatures, while the bandgap energies decrease due to the quantum size effect and the formation of rutile phase which has low bandgap energy. As a result of TG-DTA, it was found that annealing treatment at 990°C for 2 h formed a mixture of anatase and rutile through three steps: (1) the removal of physically adsorbed water (2) the decomposition of peroxo group (3) amorphous-anatase or anatase-rutile phase transformation.     

Preparation of High-Purity Lithium Carbonate Using Complexing Ion-Exchange Resins

Russian Journal of Applied Chemistry - Sorption of a series of alkaline earth and nonferrous metals (Ca, Mg, Cu, Ni, and Zn) from lithium hydrocarbonate and chloride solutions onto ion-exchange...     

川西獐牙菜及制剂中齐墩果酸的高效液相色谱测定

中药及制剂中齐墩果酸分离测定的色谱方法的色谱条件是：ＯＤＳ柱，甲醇一水（９０：１０Ｖ／Ｖ）为流动相，紫外检测器检测波长２０７ｎｍ。本研究为中药资源开发制剂的质量控制提供了简便、灵敏、准确、快速的分离测定方法。     

Sample Preparation Methods for the Determination of Chlorination Disinfection Byproducts in Water Samples

Chlorination has been widely used as a disinfection method for control of pathogens in drinking water and wastewater treatment plants. Chlorination disinfection byproducts (DBPs) are formed when organic matter is present in water, and they are harmful to human health. The main groups of compounds formed are trihalomethanes (THMs), haloacetic acids (HAAs) and haloacetonitriles (HANs). Analysis of THMs, HAAs and HANs in water samples has been reported. This paper reviews the various sample preparation methods in use for analysis of THMs, HAAs and HANs in water samples.

     

氟甲砜霉素注射液含量及其有关物质的HPLC测定

为建立测定氟甲砜霉素注射液含量的方法,采用高效液相色谱法,选用Agilent EclipseXDB-C8柱(4.6 mm×250 mm,5μm),Lab Alliance C8保护柱(4.6 mm×10 mm,5μm),流动相为(V乙腈) V(水)=35 65,流量1.0 mL.min-1,检测波长224 nm,进量样20μL,柱温为室温。结果表明,方法的线性范围为10.0～400μg.mL-1(r=0.999 6),最低检测限2.0 ng。回收率98.7%～101.2%,RSD 0.30%～1.22%(n=5)。方法简便灵敏,结果准确可靠,可用于氟甲砜霉素注射液的质量控制。     

Semi-Automated Determination of Heavy Metals in Autopsy Tissue Using Robot-Assisted Sample Preparation and ICP-MS

The endoprosthetic care of hip and knee joints introduces multiple materials into the human body. Metal containing implant surfaces release degradation products such as particulate wear and corrosion debris, metal-protein complexes, free metallic ions, inorganic metal salts or oxides. Depending on the material composition of the prostheses, a systemic exposure occurs and may result in increasing metal concentrations in body fluids and tissues especially in the case of malfunctions of the arthroplasty components. High concentrations of Cr, Co, Ni, Ti and Al affect multiple organs such as thyroid, heart, lung and cranial nerves and may lead to metallosis, intoxications, poly-neuropathy, retinopathy, cardiomyopathy and the formation of localized pseudo tumors. The determination of the concentration of metals in body fluids and tissues can be used for predicting failure of hip or knee replacements to prevent subsequent severe intoxications. A semi-automated robot-assisted measurement system is presented for the determination of heavy metals in human tissue samples using inductively coupled plasma mass spectrometry (ICP-MS). The manual and automated measurement processes were similarly validated using certified reference material and the results are compared and discussed. The automation system was successfully applied in the determination of heavy metals in human tissue; the first results are presented.     

HPLC测定复方双花口服液中绿原酸和连翘苷的含量

复方双花口服液由金银花、连翘、板蓝根等用科学方法提取有效成分精制而成 ,主治各类因金黄色葡萄球菌所致感染性疾患。绿原酸和连翘苷是该制剂中主要有效成分。我们采用十八烷基硅烷键合硅胶色谱柱 ,对该口服液中绿原酸和连翘苷含量进行同时测定 ,结果准确 ,重现性好 ,可用于复方双花口服液的质量控制     

体液直接进样高效液相色谱法测定尿中肌酐和尿酸

肌酐和尿酸是人体重要的代谢产物,二者均随尿排出.在体液中二者的含量及其比值是临床化学的重要参数.已报道的肌酐和尿酸的高效液相色谱分析方法常需要费时的样品预处理或使用复杂的柱切换设备,而且分析中还可能受其它物质的干扰,给分析工作带来麻烦.本实验室合成的聚氧乙烯交联γ.氨基两基固定相属于生物体液直接进样高效液相色谱固定相,在固定相疏水的表面键合亲水的基团,避免了体液中蛋白质变性吸附在柱中,同时利用填料的小孔径对蛋白质的体积排阻作用,使色谱柱对蛋白质不保留,而小分子物质则可以达到分离的目的.曾对该固定相考查了蛋白质回收实验,回收率达95%以上,并测定了实际样品,具有满意的柱效及柱寿命.本文利用该固定相直接进样分析了人尿中肌酐和尿酸,方法的线性范围宽,灵敏度高,准确性好,省时省力,为临床化学提供了一个有益的分析手段.     

Modern Sample Preparation Methods in Chemical Analysis

 The choice of the sample preparation method is crucial in chemical analysis, since it is often the most critical and time-consuming step of an analytical process. Some of the older methods are laborious, expensive, and offer no scope for automation. The newer sample preparation techniques can give higher yields, better sample clean-up, cost effectiveness worker safety and environmental protection. Some novel sample preparation methods are described their potential is illustrated with emphasis on bioanalytical applications.     

Determination of Glimepiride in Human Plasma by LC-MS-MS and Comparison of Sample Preparation Methods for Glimepiride

A sensitive and selective method for quantitation of glimepiride in human plasma was established using liquid chromatography-electrospray ionization tandem mass spectrometry. Three different methods for the sample preparation of glimepiride and an internal standard were investigated (liquid-liquid extraction, solid-phase extraction and protein precipitation). Glipizide was used as an internal standard. Compounds were separated on a C₁₈ column with 80% acetonitrile and 20% deionized water (adjusted to pH 3.5 with acetic acid), as mobile phase at a flow rate of 200 L min^–1. By use of multiple reaction monitoring mode in MS-MS with liquid-liquid extraction and solid-phase extraction, glimepiride and glipizide were detected without severe interference from the human plasma matrix. Glimepiride produced a protonated precursor ion ([M+H]⁺) at m/z 491 and a corresponding product ion at m/z 352, and the internal standard produced a protonated precursor ion ([M+H]⁺) at m/z 446 and a corresponding product ion at m/z 321. The limit of quantitation was 0.1 ng mL^–1, 0.5 ng mL^–1 and 1.0 ng mL^–1 when using liquid-liquid extraction, solid-phase extraction and protein precipitation, respectively. The validation, reproducibility, stability, and recovery of the different sample preparation methods were comparable and all the methods gave reliable results. The method has been successfully applied to pharmacokinetic study of glimepiride in human plasma.