敌百虫甲基对硫磷混合粉剂的高效液相色谱分析

我国新近发展的敌百虫甲基对硫磷混合粉剂(简称敌甲粉)是取代六六六制剂的品种之一。一般分析法不能同时测定两种有效成分。单独测定甲基对硫磷制剂的高效液相色谱法早有报导。Szalontai用液固吸附色谱法、氢火焰检测器,分析了敌百虫等23种有机磷农药标准物。迄今未见高效液相色谱法同时测定二者的文献。我们研究的高效液相色谱法可同时直接测定敌甲粉两种有效成分。二者分解产物不干扰分析。方法简便快速,定量结果准确。     

梯度洗脱色谱法同时测定康糖片中盐酸小檗碱、黄芩苷、格列本脲的含量

康糖片是治疗糖尿病的中西药复方制剂,主要由盐酸小檗碱、黄芩苷、格列本脲等组成。其中的单组分含量测定方法报道较多,如盐酸小檗碱有分光光度法、薄层色谱法、高效液相色谱法等;黄芩苷有比色法、薄层色谱法;格列本脲有高效液相色谱法。但同时测定上述3种组分的方法未见报道。本文报道了同时测定上述3种组     

植物中游离氨基酸的分析方法

综述了目前用于检测植物(如茶叶、蔬菜、水果、药材及烟草)中游离氨基酸的分析方法,如柱后衍生离子交换色谱法、柱前衍生反相高效液相色谱法、超高效液相色谱法、阴离子交换色谱-脉冲积分安培法、毛细管电泳法、气相色谱法和液相色谱-串联质谱法等。对这些方法的优缺点进行了讨论,同时对未来分析方法的发展提出了展望(引用文献57篇)。     

进口甲基丙烯酸甲酯中阻聚剂快速测定方法及其作用机理研究

建立了气相色谱法和高效液相色谱法快速测定甲基丙烯酸甲酯(MMA)中阻聚剂.气相色谱采用HP-INNOWAX色谱柱分离样品中杂质,液相色谱采用XDB-C18柱同时配置XDB-C18保护柱,直接对样品进行分析.结果表明,气相色语法和高效液相色谱法均具有线性关系好、回收率高等优点,方法的相对标准偏差(RSD)分别为0.53%...     

高效液相色谱法同时测定烟叶中茄尼醇和辅酶Q10的含量

高效液相色谱法同时测定烟叶中茄尼醇和辅酶Q10的含量;反相高效液相色谱;二级管阵列检测器;烟叶;茄尼醇;辅酶Q10     

环境样品中硝基苯类化合物的分析方法研究进展

主要介绍了我国近年来在环境样品中硝基苯类化合物的分析研究进展,内容包括:光度法(还原-偶氮光度法、阻抑动力学光度法、化学计量学分光光度法、人工神经网络-分光光度法)、气相色谱法(固相微萃取-毛细管气相色谱法、树脂吸附-气相色谱法、液-液微萃取气相色谱法、超声萃取-气相色谱法)、高效液相色谱法(反相高效液相色谱法、固相萃取-高效液相色谱法)和极谱法等分析方法。     

梯度洗脱色谱法同时测定康糖片中盐酸小檗咸、黄芩苷、格列本脲的含量

康糖片是治疗糖尿病的中西药复方制剂,主要由盐酸小檗碱、黄芩苷、格列本脲等组成.其中的单组分含量测定方法报道较多,如盐酸小檗碱有分光光度法[1]、薄层色谱法[2]、高效液相色谱法[3]等;黄芩苷有比色法[4]、薄层色谱法[5];格列本脲有高效液相色谱法[6].但同时测定上述3种组分的方法未见报道.本文报道了同时测定上述3种组分的高效液相色谱方法,方法简单、灵敏、回收率高、专属性强,能有效地控制药品的主成分含量,具有较强的实用价值.     

用反相高效液相色谱法纯化白细胞介素－2条件初探

用反相高效液相色谱法纯化白细胞介素－２条件初探胡明（沈阳军区军事医学研究所沈阳１１００３１）关键词反相高效液相色谱法，白细胞介素－２１前言高效液相色谱法（ＨＰＬＣ）是一项分辨率很高的液相色谱技术，具有速度快，灵敏度高、样品可回收等优点。除被广泛地应用...     

反相高效液相色谱法测定植物钩藤中钩藤碱含量

反相高效液相色谱法测定植物钩藤中钩藤碱含量;钩藤;钩藤碱;高效液相色谱法     

高效液相色谱切换波长法测定多组分体系

1引言目前植物激素常采用反相高效液相色谱法检测,但植物中激素等多种组分同时存在,单一波长不能使每个组分都在最佳检测波长下检测。本实验采用切换波长法对植物样品进行多组分检测分析,提高了检测灵敏度。采用反相高效液相色谱法(HPLC)同时测定油菜中的内源激素赤霉素(GA3)、     

HPLC determination of andrographolide in rat whole blood: study on the pharmacokinetics of andrographolide incorporated in liposomes and tablets

A sensitive and simple high-performance liquid chromatographic method with UV detection was developed and validated for the determination of andrographolide in rat whole blood. Carbamazepine was employed as internal standard and the blood sample was extracted with chloroform. Chromatographic separations were achieved on a Chromasil ODS column (250 x 4.6 mm, 5 microm). The mobile phase was consisted of methanol-water (52:48, v/v) and delivered at 0.8 mL/min. The detection wavelength was set at 225 nm. The calibration curve had a good linearity in the range 0.053-530 microg/mL in rat whole blood with its correlation coefficient being 0.996. The extraction recovery of andrographolide was ranged from 65.7 to 72.6%. The intra-day and inter-days repeatabilities were below 4.2% in terms of the percentage of relative standard deviation (RSD). The method was used to provide data on the pharmacokinetics of the drug in rats. The data obtained was processed using the 3P87 pharmacokinetic program. The results showed that the disposition of andrographolide after intravenous administration of liposomal andrographolide conformed to a two-compartment open model with alpha = 4.75 x 10(-2) +/- 2.41 x 10(-3) min(-1), beta = 3.16 x 10(-3) +/- 1.58 x 10(-4) min(-1), V(c) = 174.67 +/- 13.97 mL, k(21) = 1.60 x 10(-2) +/- 8.12 x 10(-4) min(-1), k(10) = 9.38 x 10(-3) +/- 5.62 x 10(-4) min(-1), k(12) = 2.53 x 10(-2) +/- 1.27 x 10(-3) min(-1) and AUC(0-infinity) = 1525.47 +/- 92.35 microg min/mL. For the intragastric administration of andrographolide tablets, the disposition of andrographolide followed a one-compartment open model with k(e) = 6.78 x 10(-3) +/- 3.53 x 10(-4) min(-1), k(a) = 3.69 x 10(-2) +/- 4.68 x 10(-3) min(-1), T(max) = 59.69 +/- 3.61 min, C(max) = 1.62 +/- 0.11 microg/mL, V(c) = 1056.90 +/- 83.42 mL, AUC(0-infinity) = 348.75 +/- 24.41 microg min/mL.     

高效液相色谱法测定克鲁维酵母菊芋发酵液中的乙醇,糖和有机酸类代谢成分

建立了高效液相色谱法同时分析菊芋发酵液中的乙醇和有机酸的方法.采用HPLC有机酸分析柱, 流动相为0.01 mol/L H2SO4,流速为0.5 mL/min, 以紫外和示差折光检测器作为双通道检测手段,同时对克鲁维酵母菊芋发酵液中的柠檬酸、α-酮戊二酸、葡萄糖、丙酮酸、果糖、琥珀酸、乳酸、甘油、乙酸、乙醇进行了定量分析,本方法的回收率为95.8%～109.6%;RSD为0.33%～4.0%,结果表明,本方法简单、快速、准确,适用于监控克鲁维酵母发酵产物并指导整个发酵过程条件的优化.     

A reversed-phase high-performance liquid chromatographic method for the determination of zafirlukast in pharmaceutical formulations and human plasma

Zafirlukast (ZAF) is a leukotriene receptor antagonist used in the treatment of chronic asthma. In this study, a simple and sensitive reversed-phase, high-performance liquid chromatographic method was developed for the determination of ZAF in pharmaceutical formulations and human plasma. Piribedil was used as an internal standard. Analysis was carried out on a Nucleosil C18 100 A (150 mm x 4.6 mm id, 5 Vm) column with acetonitrile-pH 3.0 acetate buffer (70 + 30, v/v) as the mobile phase at a flow rate of 0.8 mL/min. The peak was detected by an ultraviolet detector set at a wavelength of 240 nm. The retention times were about 3.9 min for piribedil and 5.8 min for ZAF. The developed method was applied to the determination of ZAF in its pharmaceutical formulation and spiked human plasma. For quantification of ZAF in spiked plasma, proteins were precipitated with ethanol before chromatographic analysis. The calibration range was linear from 49.69-437.50 ng/mL in spiked plasma. The absolute recovery from spiked plasma was 98.73 +/- 0.42% at a concentration of 254.78 ng/mL of ZAF. No endogenous substances from plasma were found to interfere.     

Validation and application of a screening method for beta2-agonists, anti-estrogenic substances and mesocarb in human urine using liquid chromatography/tandem mass spectrometry

Electrospray ionization (ESI) mass spectra of 15 anti-estrogenic substances, beta2-agonists and mesocarb were investigated in terms of fragmentation patterns. On the basis of this product ion information, a simultaneous screening method for anti-estrogenic substances, beta2-agonists and mesocarb was developed for doping control purposes. After hydrolysis, liquid-liquid extraction was adopted for the sample preparation. The recoveries for all compounds were 30 and 96%. A single liquid chromatography/tandem mass spectrometry (LC/MS/MS) analysis could be performed in 13 min for the analysis of 15 anti-estrogenic substances, beta2-agonists and mesocarb. A quantitative analysis was also validated. Inaccuracies were below +/-12% and precisions varied from 0 to 15.8%. The limit of detection was below 10 ng/mL except formestane (300 ng/mL) and aminoglutethimide (100 ng/mL). The validated method was applied for the analysis of excretion samples.     

Identification and quantification of major species of arsenic in rice

A study was undertaken to develop a method for the chemical speciation of As in rice on the basis of current knowledge in this field for use in preparing a certified reference material (CRM). Samples of the Arborio rice variety were ground to a fine powder, which was extracted under sonication with a water-methanol mixture (1 + 1, v/v). The resulting solutions were injected into a high-performance liquid chromatograph combined on-line with a quadrupole inductively coupled plasma-mass spectrometer. This hyphenated system allowed for the quantification of As species in one analytical step. Four forms of As were detected: inorganic As (III), dimethylarsinic acid (DMA), monomethylarsonic acid (MMA), and inorganic As (V) at concentrations of 88.2 +/- 7.1, 50.8 +/- 5.0, 15.2 +/- 1.7, and 51.2 +/- 3.5 ng/g, respectively. The concentration of total As was 211 +/- 7 ng/g. The limits of detection (3sigma criterion) and the quantitation (10sigma criterion) were, respectively, as follows (in ng/g): As (III), 0.095 and 0.320; As (V), 0.082 and 0.273; MMA, 0.110 and 0.367; and DMA, 0.145 and 0.480. Ten hours were needed for the extraction procedure, 6 h for the evaporation, and 30 min for quantification of the analytes. This investigation was performed in the frame of a European Commission Project on the feasibility of CRMs for As and Se species.     

Development and validation of a reverse-phase liquid chromatographic method for assay and related substances of abacavir sulfate

A simple isocratic liquid chromatographic method was developed for the determination of abacavir from its related substances and assay for the first time. This method involves the usage of C18 (Intertsil octadecyl silane-3V, 150 mm x 4.6 mm, 5 microm) column. The method was validated over the range of 0.002-0.1 mg/mL for chloro impurity, 0.005-0.1 mg/mL for amino impurity and pyrimidine impurity, and 0.005-0.2 mg/mL for abacavir. The mobile phase consists of a mixture of 10 mM ammonium acetate buffer and ACN in the ratio of 90:10. The flow rate was set at 1.0 mL/min with UV detection monitored at 214 nm. The drug substance was subjected to stress conditions of hydrolysis, oxidation, photolysis, and thermal degradation. The developed method was validated for linearity, range, precision, accuracy, and specificity. This method can be conveniently used in a quality control laboratory for routine analysis of both related substances and assay.     

1,3,5,7-四乙酰基-1,3,5,7-四氮杂环辛烷合成反应中间体的制备分离

1,3,5,7-四乙酰基-1,3,5,7-四氮杂环辛烷(TAT)是高能炸药奥克托今(HMX)重要的合成反应前体之一,1,5-二乙酰基-1,3,5,7-四氮杂环辛烷(DAPT)醋酐酰解法和乙腈甲醛小分子缩合法均能制备得到TAT.采用半制备高效液相色谱制备分离了上述两种制备方法反应原液中的六种中间体,分别是1-乙酰氧甲基-3,5,7-三乙酰基-1,3,5,7-四氮杂环辛烷、1,3,5-三乙酰基-1,3,5,7-四氮杂环辛烷、1-乙酰氧甲基-3,5,7-三乙酰基-1,3,5,7-四氮杂环辛烷、N,N’-亚甲基二乙酰胺、三乙酰胺二亚甲基三胺和四乙酰胺三亚甲基四胺,为反应机理研究提供了有力的证据.DAPT醋酐酰解法反应原液样品的最佳制备色谱条件为:正相硅胶柱(20 mm×250 mm,10～20μm),流动相:V(乙腈)∶V(甲醇)=95∶5,流速为10 mL·min-1,检测波长为215 nm,进样量为1 mL,样品浓度30 mg/mL.乙腈甲醛小分子缩合法反应原液样品的最佳制备色谱条件为:正相硅胶柱(20 mm×250 mm,10～20μm),流动相:V(乙腈)∶V(水)=90∶10,流速为10 mL·min-1,检测波长为215 nm,进样量为1 mL,样品浓度30 mg/mL.制备得到的中间体经HPLC分析知纯度均在97%以上,可直接作为结构鉴定的标准样品.     

Identification and determination of flavonoids in astragali radix by high performance liquid chromatography coupled with DAD and ESI-MS detection

A method for the analysis of flavonoids in Astragali Radix by high-performance liquid chromatography (HPLC) combined with photodiode-array detection (DAD) and an electrospray ionization (ESI)--mass spectrometry (MS) was developed. After the samples were extracted with ethanol, the optimum separation conditions for these analytes were achieved using a gradient elution system and a 2.0 x 150 mm Shimadzu VP-ODS column. Eight flavonoids were identified to exist in Astragali Radix based on their characteristic UV data and mass spectra. The concentrations of three major components in this herb--ononin, calycosin and formononetin--were determined by LC/ESI-MS in positive selective ion monitoring (SIM) mode. The calibration curves were linear in the range of 0.9~180.0 μg·mL?1 for ononin, 1.8~360.0 μg·mL?1 for calycosin and 1.4~280 μg·mL?1 for formononetin, respectively. The limits of quantification (LOQ) and detection (LOD) were 0.9 μg· mL?1 and 0.2 μg mL?1 for ononin, 1.8 μg mL?1 and 0.5 μg·mL-1 for calycosin, 1.4 μg mL?1 and 0.5 μg·mL?1 for formononetin, respectively. The standard recoveries were between 95.4~104.7%. The developed method was proven to be useful for the quantitative and qualitative analysis of flavonoid constituents in various resources of Astragali Radix.     

Characterization of a Recombinant Flocculent Saccharomyces cerevisiae Strain that Co-ferments Glucose and Xylose: I. Influence of the Ratio of Glucose/Xylose on Ethanol Production

Glucose/xylose mixtures (90 g/L total sugar) were evaluated for their effect on ethanol fermentation by a recombinant flocculent Saccharomyces cerevisiae, MA-R4. Glucose was utilized faster than xylose at any ratio of glucose/xylose, although MA-R4 can simultaneously co-ferment both sugars. A high percentage of glucose can increase cell biomass production and therefore increase the rate of glucose utilization (1.224 g glucose/g biomass/h maximum) and ethanol formation (0.493 g ethanol/g biomass/h maximum). However, the best ratio of glucose/xylose for the highest xylose consumption rate (0.209 g xylose/g biomass/h) was 2:3. Ethanol concentration and yield increased and by-product (xylitol, glycerol, and acetic acid) concentration decreased as the proportion of glucose increased. The maximum ethanol concentration was 41.6 and 21.9 g/L after 72 h of fermentation with 90 g/L glucose and 90 g/L xylose, respectively, while the ethanol yield was 0.454 and 0.335 g/g in 90 g/L glucose and 90 g/L xylose media, respectively. High ethanol yield when a high percentage of glucose is available is likely due to decreased production of by-products, such as glycerol and acetic acid. These results suggest that ethanol selectivity is increased when a higher proportion of glucose is available and reduced when a higher proportion of xylose is available.     

银莱汤中主要成分的UPLC多波长宽动态测定及质量评价研究

采用超高效液相色谱(UPLC)定量测定银莱汤中10种有效成分的含量并用于其质量评价。采用Waters ACQUITY UPLC HSS T3色谱柱(2.1 mm×100 mm,1.8μm),以0.1%甲酸水溶液-0.1%甲酸乙腈为流动相梯度洗脱,3波长切换(0~10 min,320 nm;10~16 min,350 nm;16~30 min,320 nm)测定。结果表明,该方法可在30 min内实现银莱汤中10种有效成分的基线分离,10种成分在各自质量浓度范围内线性关系良好(r≥0.9992),检出限为0.0188~0.0750μg·mL-1,定量下限为0.0625~0.250μg·mL-1。检测得到银莱汤中10种成分的平均含量为0.204~38.129 mg·g-1,其中黄芩苷的含量最高,槲皮苷的含量最低。将该方法用于3批样品分析,所测成分含量稳定、一致性好。该文建立的分析指标相对全面、合理可行,能更好地表征及评价银莱汤质量。