您现在的位置:首页>美国卫生研究院文献>Analytical Chemistry Insights

期刊信息

  • 期刊名称:

    -

  • 刊频: Irregular
  • NLM标题:
  • iso缩写: -
  • ISSN: -

年度选择

更多>>

  • 排序:
  • 显示:
  • 每页:
全选(0
<3/6>
110条结果
  • 机译 快速指示RP-HPLC法测定药物片剂中盐酸倍他洛尔的含量
    摘要:A stability-indicating reversed-phase high performance liquid chromatography (RP-HPLC) method was developed for the determination of betaxolol hydrochloride, a drug used in the treatment of hypertension and glaucoma. The desired chromatographic separation was achieved on a Nucleosil C18, 4 μm (150 × 4.6 mm) column, using isocratic elution at a 220 nm detector wavelength. The optimized mobile phase consisted of a 0.02 M potassium dihydrogen phosphate: methanol (40:60, v/v, pH 3.0 adjusted with o- phosphoric acid) as solvent. The flow rate was 1.6 mL/min and the retention time of betaxolol hydrochloride was 1.72 min. The linearity for betaxolol hydrochloride was in the range of 25 to 200 μg/mL. Recovery for betaxolol hydrochloride was calculated as 100.01%–101.35%. The stability-indicating capability was established by forced degradation experiments and the separation of unknown degradation products. The developed RP-HPLC method was validated according to the International Conference on Harmonization (ICH) guidelines. This validated method was applied for the estimation of betaxolol hydrochloride in commercially available tablets.
  • 机译 实验设计在柱前衍生化中使用HPLC进行妥布霉素分析的荧光检测—在眼药水和人体血浆中的应用
    摘要:A novel, selective, and sensitive reversed phase high-performance liquid chromatography (HPLC) method coupled with fluorescence detection has been developed for the determination of tobramycin (TOB) in pure form, in ophthalmic solution and in spiked human plasma. Since TOB lacks UV absorbing chromophores and native fluorescence, pre-column derivatization of TOB was carried out using fluorescamine reagent (0.01%, 1.5 mL) and borate buffer (pH 8.5, 2 mL). Experimental design was applied for optimization of the derivatization step. The resulting highly fluorescent stable derivative was chromatographed on C18 column and eluted using methanol:water (60:40, v/v) at a flow rate of 1 mL min−1. A fluorescence detector (λex 390 and λem 480 nm) was used. The method was linear over the concentration range 20–200 ng mL−1. The structure of the fluorescent product was proposed, the method was then validated and applied for the determination of TOB in human plasma. The results were statistically compared with the reference method, revealing no significant difference.
  • 机译 汞膜电极吸附溶出伏安法测定稀释碱性电解质中抗逆转录病毒药物阿昔洛韦。
    摘要:This paper describes a stripping method for the determination of acyclovir at the submicromolar concentration level. This method is based on controlled adsorptive accumulation of acyclovir at thin-film mercury electrode, followed by a linear cyclic scan voltammetry measurement of the surface species. Optimal experimental conditions include a NaOH solution of 2.0 × 10−3 mol L−1 (supporting electrolyte), an accumulation potential of −0.40 V, and a scan rate of 100 mV s−1. The response of acyclovir is linear over the concentration range 0.02 to 0.12 ppm. For an accumulation time of 4 minutes, the detection limit was found to be 0.42 ppb (1.0 × 10−9 mol L−1). More convenient methods to measure the acyclovir in presence of the didanosine, efavirenz, nevirapine, nelfinavir, lamivudine, and zidovudine were also investigated. The utility of this method is demonstrated by the presence of acyclovir together with Adenosine triphosphate (ATP) or DNA.
  • 机译 天竺葵植物材料中存在1,3-二甲基戊胺(1,3-DMAA)的证据
    摘要:1,3-Dimethylamylamine (1,3-DMAA) is an aliphatic amine with stimulant properties that are reportedly found naturally only in geranium plants (Pelargonium graveolens). The presence of 1,3-DMAA in geranium plants was first reported in a paper published in 1996, but some have questioned the identification of 1,3-DMAA in that study. Since then, a number of additional studies have been published, largely reporting the absence of 1,3-DMAA in geranium plants and commercial geranium oils. However, in two recent studies, 1,3-DMAA was detected in geranium plant tissues and a geranium oil sample using a simplified extraction approach on tissues and oil sourced from China. Whether or not 1,3-DMAA is found naturally in plants has significant implications as to how commercial products containing 1,3-DMAA are regulated by the US Food and Drug Administration. In this paper, differences in source materials, extraction procedures, and analytical approaches are reviewed in an attempt to rationalize the apparently conflicting evidence for the presence of 1,3-DMAA in geranium plant materials.
  • 机译 牙买加曼彻斯特教区晚中新世或上新世鸟粪中有机物的生化特征
    摘要:The biogeochemical fate of organic matter (OM) entering soils is an important issue that must be examined to better understand its roles in nitrogen cycling and as a natural modulator of soil-atmospheric carbon fluxes. Despite these critical roles, there are uncertainties in estimating the contribution of this feedback mechanism due in part to a lack of molecular-level information regarding the origin and labile and refractory inventories of OM in soils. In this study, we used a multi-analytical approach to determine molecular-level information for the occurrence and stabilization of OM in a bird guano concretion of the Late Miocene or Pliocene age in Jamaica. We determined the specific organic structures persisting in the concretion and the possible contribution of fossil organic matter to the OM pool in modern environments. Our results indicate that aliphatic species, presumably of a highly polymethylenic nature [(CH2)n], may significantly contribute to the stable soil-C pool. Although not as significant, proteins and carbohydrates were also enriched in the sample, further suggesting that fossil organic matter may contribute to carbon and nitrogen pools in present day soil organic matter.
  • 机译 确定pKa值的方法的发展
    摘要:The acid dissociation constant (pKa) is among the most frequently used physicochemical parameters, and its determination is of interest to a wide range of research fields. We present a brief introduction on the conceptual development of pKa as a physical parameter and its relationship to the concept of the pH of a solution. This is followed by a general summary of the historical development and current state of the techniques of pKa determination and an attempt to develop insight into future developments. Fourteen methods of determining the acid dissociation constant are placed in context and are critically evaluated to make a fair comparison and to determine their applications in modern chemistry. Additionally, we have studied these techniques in light of present trends in science and technology and attempt to determine how these trends might affect future developments in the field.
  • 机译 扑热息痛危险性杂质存在下RP-LC和TLC光度法测定扑热息痛和苯溴胺的含量及其在制药中的应用
    摘要:Two simple, accurate and reproducible methods were developed and validated for the simultaneous determination of paracetamol (PARA) and pamabrom (PAMB) in pure form and in tablets. The first method was based on reserved-phase high-performance liquid chromatography, on a Thermo Hypersil ODS column using methanol:0.01 M sodium hexane sulfonate:formic acid (67.5:212.5:1 v/v/v) as the mobile phase. The flow rate was 2 mL/min and the column temperature was adjusted to 35 °C. Quantification was achieved with UV detection at 277 nm over concentration range of 100–600 and 4–24 μg/mL, with mean percentage recoveries were found to be 99.90 ± 0.586 and 99.26 ± 0.901 for PARA and PAMB, respectively. The second method was based on thin-layer chromatography separation of PARA and PAMB followed by densitometric measurement of the spots at 254 nm and 277 nm for PARA and PAMB respectively. Separation was carried out on aluminum sheet of silica gel 60F254 using dichloromethane:methanol:glacial acetic acid (7.5:1:0.5 v/v/v) as the mobile phase over concentration range of 1–10 and 0.32–3.20 μg per spot, with mean percentage recovery of 100.52 ± 1.332 and 99.71 ± 1.478 for PARA and PAMB, respectively. The methods retained their accuracy in presence of up to 50% of P-aminophenol and could be successfully applied in tablets.
  • 机译 两种市售便携式拉曼系统的评估
    摘要:Raman spectroscopy and surface enhanced Raman spectroscopy (SERS) have many attributes that make them attractive for field detection of environmental contaminants, industrial process control, as well as materials detection/identification in agriculture, pharmaceuticals, law enforcement/first responders, geology, and archeology. However, portable, robust, inexpensive Raman systems are required for these applications. In this communication, the performances of two commercially available, portable Raman systems are evaluated.
  • 机译 RP-LC法测定肉桂酸报道的降解产物中肉桂酸/吡乙酰胺和肉桂酸/庚胺基乙酰基亚麻酸酯的开发和验证
    摘要:Specific stability indicating reverse-phase liquid chromatography (RP-LC) assay method (SIAM) was developed for the determination of cinnarizine (Cinn)/piracetam (Pira) and cinnarizine (Cinn)/heptaminol acefyllinate (Hept) in the presence of the reported degradation products of Cinn. A C18 column and gradient mobile phase was applied for good resolution of all peaks. The detection was achieved at 210 nm and 254 nm for Cinn/Pira and Cinn/Hept, respectively. The responses were linear over concentration ranges of 20–200, 20–1000 and 25–1000 μgmL−1 for Cinn, Pira, and Hept respectively. The proposed method was validated for linearity, accuracy, repeatability, intermediate precision, and robustness via statistical analysis of the data. The method was shown to be precise, accurate, reproducible, sensitive, and selective for the analysis of Cinn/Pira and Cinn/Hept in laboratory prepared mixtures and in pharmaceutical formulations.
  • 机译 荧光光谱-高效液相色谱-荧光光谱法同时测定混合液中苯磺酸氨氯地平和阿托伐他汀钙。
    摘要:Caduet tablets are novel prescription drug that combines amlodipine besylate (AM) with atorvastatin calcium (AT). A spectrofluorimetric and an HPLC-fluorescence detection methods were developed for simultaneous determination of both drugs in tablets. In the spectrofluorimetric method, native fluorescence of AM and AT were measured in methanol at 442 and 369 nm upon excitation at 361 and 274 nm, respectively. The emission spectrum of each drug reveals zero value at the emission wavelength of the other drug, thus allowing their simultaneous determination without interference. In the HPLC method, separation of AM and AT was achieved within 8 minutes on a C18 column using acetonitrile:phosphate buffer (0.015 M, pH 3) (45:55, v/v) as the mobile phase. Fluorescence detection was carried out using excitation wavelengths 361 and 274 nm and emission wavelengths 442 and 378 nm for AM and AT, respectively. Excellent linearity was observed. Careful validation proved advantages of the new methods: high sensitivity, accuracy, selectivity and suitability for quality control laboratories.
  • 机译 基于鼠尾草(Salvia officinalis L.)的凉茶和Tin剂的全程控制,使用NMR光谱对具有有益和不利作用的化合物
    摘要:A methodology that utilizes 1H-NMR spectroscopy has been developed to simultaneously analyze toxic terpenes (thujone and camphor), major polyphenolic compounds, the total antioxidant capacity (ORAC) and the Folin-Ciocalteu (FC) index in foods and medicines containing sage. The quantitative determination of rosmarinic acid (limit of detection (LOD) = 10 mg/L) and total thujone (LOD = 0.35 mg/L) was possible using direct integration of the signals. For other parameters (derivatives of rosmarinic acid, carnosol and flavone glycosides, ORAC and FC index), chemometric regression models obtained separately for alcohol-based tinctures (R2 = 0.94–0.98) and aqueous tea infusions (R2 = 0.79–0.99) were suitable for screening analysis. The relative standard deviations for authentic samples were below 10%. The developed methodology was applied for the analysis of a wide variety of sage products (n = 108). The total thujone content in aqueous tea infusions was found to be in the range of not detectable (nd) to 37.5 mg/L (average 9.2 mg/L), while tinctures contained higher levels (range nd—409 mg/L, average 107 mg/L). The camphor content varied from 2.1 to 43.7 mg/L in aqueous infusions and from not detectable to 748 mg/L in tinctures (averages were 14.1 and 206 mg/L, respectively). Phenolic compounds were also detected in the majority of the investigated products. 1H-NMR spectroscopy was proven to have the ability to holistically control all important adverse and beneficial compounds in sage products in a single experiment, considerably saving time, resources and costs as NMR replaces four separate methodologies that were previously needed to analyze the same parameters.
  • 机译 两种色谱法测定某些偏头痛药物
    摘要:Two stability indicating chromatographic methods were proposed for the determination of almotriptan, eletriptan, and rizatriptan, in presence of their acid degradation products. The first method is a quantitative densitometric thin layer chromatography. The developing systems were; acetonitrile: methanol: dichloromethane: ammonia (10:6:3:1 v/v), ethyl acetate: methanol: ammonia (15:4:1 v/v), and methanol: acetonitrile: ammonia (9:4:1 v/v) for almotriptan, eletriptan and rizatriptan respectively. The TLC plates were scanned at 235 nm. Linear relationships were obtained over concentration ranges (5–50 μg/spot) for almotriptan and rizatriptan, and (5–60 μg/spot) for eletriptan. The second method based on the separation and determination of the studied drugs, using RP-HPLC technique. The separation was achieved on C18 Hypersil column, elution was carried out using phosphate buffer pH 3: methanol: acetonitrile (2: 1:1 v/v) at flow rate 2 mL/min and UV detection at 235 nm. Linear relationships were obtained over concentration ranges (10–200 μg/mL) for almotriptan and eletriptan, and (10–180 μg/mL) for rizatriptan. The chromatographic methods were successfully applied for the determination of each of the studied drugs in pure form, tablet form, and in laboratory prepared mixtures with their acid degradation products.
  • 机译 基于络合平衡方程的血清电离钙计算模型
    摘要:Measurement of ionized calcium is more important than measurement of total calcium in serum samples. In the present study, equations were derived from complexation and acid dissociation equilibrium equations, and were used to determine the concentration of ionized calcium from the observed serum concentrations of total calcium, albumin, total protein, and inorganic phosphate. The ionized calcium concentration was calculated in 67 serum samples from healthy subjects and 34 outpatients previously identified as having abnormal serum calcium levels. The correlation coefficient between our method (y) and the calcium-ion-selective electrode method (x) was 0.953 and the linear regression equation was y = 0.97x at pH 7.4 with a factor of α = 0.21, which was based on the differences between the concentrations of calcium phosphorus compounds obtained by the electrode method and by calculation. The developed calculation is as useful and accurate as the electrode method, and therefore extremely useful for clinical diagnoses.
  • 机译 毛细管区带电泳同时测定药物制剂中西他列汀和二甲双胍的含量及其在人体血浆分析中的应用
    摘要:A novel, quick, reliable and simple capillary zone electrophoresis CZE method was developed and validated for the simultaneous determination of sitagliptin (SG) and metformin (MF) in pharmaceutical preparations. Separation was carried out in fused silica capillary (50.0 cm total length and 43.0 cm effective length, 49 μm i.d.) by applying a potential of 15 KV (positive polarity) and a running buffer containing 60 mM phosphate buffer at pH 4.0 with UV detection at 203 nm. The samples were injected hydrodynamically for 3 s at 0.5 psi and the temperature of the capillary cartridge was kept at 25 °C. Phenformin was used as internal standard (IS). The method was suitably validated with respect to specificity, linearity, limit of detection and quantitation, accuracy, precision, and robustness. The method showed good linearity in the ranges of 10–100 μg/mL and 50–500 μg/mL with limits of detection of 0.49, 2.11 μg/mL and limits of quantification of 1.48, 6.39 μg/mL for SG and MF, respectively. The proposed method was successfully applied for the analysis of the studied drugs in their synthetic mixtures and co-formulated tablets without interfering peaks due to the excipients present in the pharmaceutical tablets. The method was further extended to the in-vitro determination of the two drugs in spiked human plasma. The estimated amounts of SG/MF were almost identical with the certified values, and their percentage relative standard deviation values (% R.S.D.) were found to be ≤1.50% (n = 3). The results were compared to a reference method reported in the literature and no significant difference was found statistically.
  • 机译 液相色谱串联质谱法鉴定和定量天竺葵中的二甲基戊胺
    摘要:A sensitive and reliable method of liquid chromatography–electrospray ionization/tandem mass spectrometry (LC-ESI/MS/ MS) was developed and validated for determining 1,3-dimethylamylamine (1,3-DMAA) and 1,4-dimethylamylamine (1,4-DMAA) in geranium plants (Pelargonium graveolens). The sample was extracted with 0.5 M HCl and purified by liquid-liquid partition with hexane. The parameters for reverse-phase (C18) LC and positive ESI/MS/MS were optimized. The matrix effect, specificity, linearity, precision, accuracy and reproducibility of the method were determined and evaluated. The method was linear over a range of 0.10–10.00 ng/mL examined, with R2 of 0.99 for both 1,3-DMAA and 1,4-DMAA. The recoveries from spiked concentrations between 5.00–40.00 ng/g were 85.1%–104.9% for 1,3-DMAA, with relative standard deviation (RSD) of 2.9%–11.0%, and 82.9%–101.8% for 1,4-DMAA, with RSD of 3.2%–11.7%. The instrument detection limit was 1–2 pg for both DMAAs. The quantification limit was estimated to be 1–2 ng/g for the plant sample. This method was successfully applied to the quantitative determination of 1,3- and 1,4-DMAA in both geranium plant and geranium oil.
  • 机译 高效液相色谱-串联质谱法在ng / g浓度下对天竺葵植物中1,3-DMAA和1,4-DMAA的分析和确认
    摘要:1,3-Dimethylamylamine (1,3-DMAA) is a stimulant commercially sold in a variety of dietary supplements as a chemical species derived from geranium plants (Pelargonium graveolens). Whether 1,3-DMAA naturally occurs in geranium plants or other dietary ingredients, it has important regulatory and commercial ramifications. However, the analysis of 1,3-DMAA in geranium plants is not trivial due to low concentrations and a complex environmental matrix, requiring high selectivity and sensitivity. An extraction method combined with high performance liquid chromatography and tandem mass spectrometry is used to determine 1,3-DMAA and 1,4-dimethylamylamine (1,4-DMAA) concentrations in geranium plants with both external calibration and standard addition method. Samples from the Changzhou, Kunming, and Guiyang regions of China during both winter and summer were analyzed for 1,3-DMAA and 1,4-DMAA. The diastereomer ratios of the 1,3-DMAA stereoisomers of a racemic standard and the extracted plant were also quantified.
  • 机译 评估第二代木质素分析的基质辅助激光解吸/电离质谱
    摘要:Matrix-Assisted Laser Desorption/Ionization time-of-flight (MALDI-TOF) mass spectrometry is evaluated as an elucidation tool for structural features and molecular weights estimation of some extracted herbaceous lignins. Optimization of analysis conditions, using a typical organic matrix, namely α-cyano-4-hydroxycinnamic acid (CHCA), in combination with α-cyclodextrin, allows efficient ionization of poorly soluble lignin materials and suppression of matrix-related ions background. Analysis of low-mass fragments ions (m/z 100–600) in the positive ion mode offers a “fingerprint” of starting lignins that could be a fine strategy to qualitatively identify principal inter-unit linkages between phenylpropanoid units. The molecular weights of lignins are estimated using size exclusion chromatography and compared to MALDI-TOF-MS profiles. Miscanthus (Miscanthus x giganteus) and Switchgrass (Panicum Virgatum L.) lignins, recovered after a formic acid/acetic acid/water process or aqueous ammonia soaking, are selected as benchmarks for this study.
  • 机译 铬铁菁R络合物络合分光光度法测定of
    摘要:A novel and sensitive floatation-spectrophotometric method is presented for determination of trace amounts of thorium in water samples. The method is based on the ion-associated formation between thorium, Eriochrome cyanine R and Brij-35 at pH = 4 media. The complex was floated in the interface of the aqueous phase and n-hexane by vigorous shaking. After removing the aqueous phase the floated particles were dissolved in methanol and the absorbance was measured at 607 nm. The influence of different important parameters such as Eriochrome cyanine R and surfactants concentration, pH, volume of n-hexane, standing time and interfering ions were evaluated. Under optimized conditions the calibration graph was linear in the range of 6–230 ng mL−1 of thorium with a correlation coefficient of 0.9985. The limit of detections (LOD), based on signal to noise ratio (S/N) of 3 was 1.7 ng mL−1. The relative standard deviations for determination of 150 and 30 ng ml−1 of thorium were 3.26 and 4.41%, respectively (n = 10). The method showed a good linearity, recoveries, as well as some advantages such as sensitivity, simplicity, affordability and a high feasibility. The method was successfully applied to determine thorium in different water and urine samples.
  • 机译 柱前衍生技术用于紫外检测检测美罗培南药物中乙二胺四乙酸的有效反相高效液相色谱法
    摘要:This paper deals with development and validation of a high performance liquid chromatographic method for the quantitative determination of disodium EDTA (Ethylenediaminetetraacetic acid) in Meropenem active pharmaceutical ingredient (API). EDTA was derivatized with Ferric chloride solution by heating at 70 °C in water bath for about 20 minutes and the chromatographic separation achieved by injecting 100 μL of the derivatized mixture into a Waters HPLC system with photodiode array detector using a Phenomenex Luna C18(2) column (250 × 4.6 mm), 5 μ. The mobile phase consisting of 5% methanol and 95% of 0.7 g/L solution of Tetra butyl ammonium bromide and 4.6 g/L solution of sodium acetate trihydrate in water (pH adjusted to 4.0 with the help of acetic acid glacial) and a flow rate of 1 milliliter/minute. EDTA eluted at approximately 6 minutes. The method was suitably validated with respect to specificity, linearity of response, precision, accuracy, ruggedness, stability in analytical solution, limit of quantitation and detection and robustness for its intended use.
  • 机译 浮选-分光光度法测定痕量铅。
    摘要:The present study describes a simple and highly selective method for separation, preconcentration and spectrophotometric determination of extremely low concentrations of lead. It is based on flotation of a complex of Pb2+ ions and Alizarin yellow between aqueous and n-hexane interface at pH = 6. The proposed procedure is also applied for determination of lead in both tap water and prepared sea water samples. Beer’s Law was obeyed over the concentration range of 3.86 × 10–8 To 8.20 × 10–7 molL−1 (8–170 ngmL−1) with an apparent molar absorptivity of 1.33 × 106 molL−1 cm−1 for a 100 mL aliquot of the water sample. The detection limit (n = 10) was 8.7 × 10–9 molL−1 (1.0 ngmL−1) and the Relative standard deviation (R.S.D), (n = 10) for 7.2 × 10–7 molL−1 (150 ngmL−1) of Pb (II) was 4.36%. A notable advantage of the method is that the determination of Pb (II) is free from the interference of almost all cations and ions found in the environment and waste water samples. The determination of Pb (II) in tap and synthetic seawater samples was also carried out by the present method. The results were satisfactorily comparable so that the applicability of the proposed method was confirmed to the real samples.

客服邮箱:kefu@zhangqiaokeyan.com

京公网安备:11010802029741号 ICP备案号:京ICP备15016152号-6 六维联合信息科技 (北京) 有限公司©版权所有
  • 客服微信

  • 服务号