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高效液相色谱法测定糙米粉中的维生素 总被引:7,自引:1,他引:7
高效液相色谱法测定糙米粉中的维生素吴红京,唐根源,王勇(中国科学院福建物质结构研究所福州350002)(福建药品检验所福州350001)1前言众所周知,糙米粉有很高的营养价值,含有人体必需的多种维生素。用高效液相色谱法(HPLC)和薄层色谱法(TLC... 相似文献
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填充毛细管液相色谱—毛细管气相色谱在线联用分析柴油全组成 总被引:5,自引:0,他引:5
采用填充毛细管液相色谱(PC-HPLC)与毛管气相色谱(CGC)在线联用技术分析柴油全组分。半填充硅胶、半填充氨基的PC-HPLC柱(0.32mm i.d)用于样品族分离(烷烃、单环芳烃、双环芳烃、三环芳烃和胶质)。经PC-HPLC分离后的各族组分(峰体积小于30μL)被依次存放在多位储存接口内,然后分别转入GC作单个组分定量分析,可得出各族组分的相对含量及烷烃的碳数的正异构分布。该方法是分析柴油 相似文献
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反相高效液相色谱法同时测定法莫替丁及其相关物质的含量 总被引:1,自引:0,他引:1
1 引 言 法莫替丁(famotidine)是日本山之内制药株式会社开发的继西咪替丁、雷尼替丁后的第三代组胺受体拮抗剂,其抑制胃酸分泌比前两者强而持久。日本药典、美国药典及我国部颁标准规定以高氯酸非水滴定法测定其含量;对其相关物质采用薄层色谱法(TLC)。此类法定方法的测定准确度及重现性不甚理想,为此,关衍军等对我国部颁标准作了改进;李思明等曾报道了其片剂的紫外分光光度法,沈向忠等用高效液相色谱法(HPLC)测定了其片剂,但都无涉及其原药与相关物质的检测方法。本文研究了法莫替丁原药及其相关物质在RP-HPL… 相似文献
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柱切换高效液相色谱法在生物样品中的应用 总被引:1,自引:0,他引:1
评述了柱切换高效液相色谱法(CSHPLC)在生物样品分析中的应用进展.分别对柱切换装置,血样、尿样提取液中被测组分浓度的测定,在线浓缩样品技术以及CSHPLC的联用进行了介绍. 相似文献
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HPLC测定煤焦油中极性化合物的研究 总被引:7,自引:0,他引:7
应用高效液相色谱以正相-HPLC配以反冲(BF)技术,测定了煤焦油中极性化合物的总量。以反相(RF)-HPLC辅以制备液体色谱研究了极性段份的制备及典型极性化合物的分析,文中分析的实样由山西省一些焦化厂提供。 相似文献
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Comparison of high performance TLC and HPLC for separation and quantification of chlorogenic acid in green coffee bean extracts 总被引:1,自引:0,他引:1
Urakova IN Pozharitskaya ON Shikov AN Kosman VM Makarov VG 《Journal of separation science》2008,31(2):237-241
Two chromatographic methods, high-performance TLC (HPTLC) and HPLC, were developed and used for separation and quantitative determination of chlorogenic acid in green coffee bean extracts. For HPTLC silica gel Kieselgel 60 F 254 plates with ethyl acetate/dichlormethane/formic acid/acetic acid/water (100:25:10:10:11, v/v/v/v/v) as mobile phase were used. Densitometric determination of chlorogenic acid by HPTLC was performed at 330 nm. A gradient RP HPLC method was carried out at 330 nm. All necessary validation tests for both methods were developed for their comparison. There were no statistically significant differences between HPLC and HPTLC for quantitative determination of chlorogenic acid according to the test of equality of the means. 相似文献
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Webster L Walsham P Ahmed Y Richards S Hay S Heath M Moffat CF 《Journal of separation science》2006,29(9):1205-1216
A method was developed for the determination of the major storage lipids, wax ester and triglycerides, in the copepod Calanus finmarchicus. A variation of the Folch method was used to extract the lipid. The method was scaled down to enable the extraction of either pooled (-1 mg) or individual (approximately 200 microg) copepods. The major lipid classes were identified using TLC and quantified using HPLC coupled with evaporative light scattering detection. Analysis of laboratory reference materials indicated that this method underestimated the minor triglyceride component, but gave a good estimate of the major wax ester component. The fatty acid and fatty alcohol composition of the C. finmarchicus were determined following trans-esterification of the lipid extract in methanol. Fatty acids and fatty alcohols were initially identified by comparison with authentic standard and by mass spectroscopy. Using GC with flame ionisation detection the normalised area percentage of the fatty alcohols and fatty acid methyl esters was determined simultaneously in one run for either pooled or individual copepod samples. These methods were applied to C. finmarchicus collected from the Irminger Sea, North Atlantic in 2001 and 2002. 相似文献
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Abdel-Fattah LS El-Sherif ZA Kilani KM El-Haddad DA 《Journal of AOAC International》2010,93(4):1180-1191
Three stability-indicating assay methods were developed for the determination of tropisetron in a pharmaceutical dosage form in the presence of its degradation products. The proposed techniques are HPLC, TLC, and first-derivative spectrophotometry (1D). Acid degradation was carried out, and the degradation products were separated by TLC and identified by IR, NMR, and MS techniques. The HPLC method was based on determination of tropisetron in the presence of its acid-induced degradation product on an RP Nucleosil C18 column using methanol-water-acetonitrile-trimethylamine (65 + 20 + 15 + 0.2, v/v/v/v) mobile phase and UV detection at 285 nm. The TLC method was based on the separation of tropisetron and its acid-induced degradation products, followed by densitometric measurement of the intact spot at 285 nm. The separation was carried out on silica gel 60 F254 aluminum sheets using methanol-glacial acetic acid (22 + 3, v/v) mobile phase. The 1D method was based on the measurement of first-derivative amplitudes of tropisetron in H2O at the zero-crossing point of its acid-induced degradation product at 271.9 nm. Linearity, accuracy, and precision were found to be acceptable over concentration ranges of 40-240 microg/mL, 1-10 microg/spot, and 6-36 micro/mL for the HPLC, TLC, and 1D methods, respectively. The suggested methods were successfully applied for the determination of the drug in bulk powder, laboratory-prepared mixtures, and a commercial sample. 相似文献
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Thin-layer chromatographic scanner, spectrophotometric and high-performance liquid chromatographic methods for the determination of colchicine 总被引:4,自引:0,他引:4
One high-performance liquid chromatographic (HPLC) and two thin-layer chromatographic (TLC) methods are proposed for the determination of colchicine in crude drugs and pharmaceutical preparations. The TLC scanner method is based on measurement of the absorbance of the separated colchicine spot; alternatively, after scraping the spot from the plate and elution the absorbance can be measured spectrophotometrically. The HPLC assay was carried out isocratically on a reversed-phase column using MeOH-H2O (60 + 40). The recoveries were 99.2 +/- 1.23, 99.1 +/- 1.12 and 99.1 +/- 2.01% for the TLC scanner, spectrophotometric and HPLC methods, respectively. The methods were shown to be sensitive and specific and can be used as an alternative to the pharmacopoeial methods having been applied to the determination of colchicine in corms of Merendera persica and in three pharmaceutical preparations. 相似文献
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Molinier V Fenet B Fitremann J Bouchu A Queneau Y 《Journal of colloid and interface science》2005,286(1):360-368
The micellization of pure monosubstituted sucrose fatty acid esters in water, namely sucrose octanoate, sucrose decanoate, sucrose laurate, sucrose dodec-5-cis-enoate, sucrose myristate, and sucrose palmitate, has been investigated by means of two NMR methods, pulsed field gradient spin-echo NMR (PFGSE-NMR), giving access to the self-diffusion coefficients of free molecules and micelles in solution, and the ERETIC method (electronic reference to access in vivo concentrations) for the measurement of concentrations by external calibration of a synthetic NMR signal. The early micellar regions and, when possible, the premicellar regions were investigated. By this method, we obtained the hydrodynamic radii of micelles, displaying a linear progression in relation to the chain length and an accurate determination of critical micellar concentration (CMC) for each sucrose ester. The effect of the regiochemistry of fatty chain grafting has been investigated, showing special behavior for 1'-O-sucrose palmitate. 相似文献
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D. Agbaba A. Mihajlovic P. Beljanski D. Zivanov-Stakic S. Vladimirov 《Chromatographia》1997,45(1):145-148
Summary TLC and HPLC methods for the determination of the preservative, 8-hydroxyquinoline sulfate in PPD-T tuberculin solution were
developed. The planar chromatography method involved separation of 8-hydroxyquinoline sulfate on a TLC plate using a butyl-acetate:
formic acid: 2-propanol mobile phase, detection and quantitation by densitometric scanning. The HPLC method was on a LiChrosorb
RP-18 column with acetonitrile-water (65:35 v/v) mobile phase, adjusted to pH 3.05 by phosphoric acid. Linearity, reproducibility
and accuracy were found to be satisfactory. Under selected conditions, the limit of detection (LOD) of both methods was similar-about
25 ng.
Presented at the 21st ISC held in Stuttgart, Germany, 15th–20th September, 1996 相似文献
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Stability‐indicating chromatographic methods for determination of flecainide acetate in the presence of its degradation products; isolation and identification of two of its impurities 下载免费PDF全文
Nariman A. El‐Ragehy Nagiba Y. Hassan Mahmoud A. Tantawy Mohamed Abdelkawy 《Biomedical chromatography : BMC》2016,30(10):1541-1548
In this work, two stability‐indicating chromatographic methods have been developed and validated for determination of flecainide acetate (an antiarrhythmic drug) in the presence of its degradation products (flecainide impurities; B and D). Flecainide acetate was subjected to a stress stability study including acid, alkali, oxidative, photolytic and thermal degradation. The suggested chromatographic methods included the use of thin layer chromatography (TLC‐densitometry) and high‐performance liquid chromatography (HPLC). The TLC method employed aluminum TLC plates precoated with silica gel G.F254 as the stationary phase and methanol–ethyl acetate–33% ammonia (3:7:0.3, by volume) as the mobile phase. The chromatograms were scanned at 290 nm and visualized in daylight by the aid of iodine vapor. The developed HPLC method used a RP‐C18 column with isocratic elution. Separation was achieved using a mobile phase composed of phosphate buffer pH 3.3–acetonitrile–triethylamine (53:47:0.03, by volume) at a flow rate of 1.0 mL/min and UV detection at 292 nm. Factors affecting the efficiency of HPLC method have been studied carefully to reach the optimum conditions for separation. The developed methods were validated according to the International Conference on Harmonization guidelines and were applied for bulk powder and dosage form. Copyright © 2016 John Wiley & Sons, Ltd. 相似文献
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Summary A specific and sensitive reverse-phase HPLC method for the quantitative determination of ascorbic acid and antioxidant synergists (1-tartaric acid, citric acid, lactic acid as lithium lactate and EDTA) in fatty pharmaceuticals, cosmetics and food has been developed. Two extraction procedures were used; treatment with hot water, and extraction with water from a hexane dilution of the product. No significant differences between the two procedures were found (p<0.05), except for ascorbic acid. Quantitative determinations were performed using a C-18 column and sulfuric acid (pH 1.95) mobile phase. With detection, at 210 nm, lactic acid overlapped with ascorbic acid, but the former could be readily identified by TLC. Ascorbic acid was detected at 254 nm, when lactic acid (as lithium lactate) did not interfere in the analysis. Mean recoveries for tartaric, citric and lactic acids were in the range 96–101%. 相似文献
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Determination of aflatoxins in food products by chromatography. 总被引:1,自引:0,他引:1
Several chromatographic methods for the determination of aflatoxins in agricultural and food products are reviewed. During the past two decades, identification and determination of aflatoxins were done by thin-layer chromatography (TLC) because it was easy, fast and inexpensive. However, high-performance liquid chromatography (HPLC) using fluorescence detection is now the method of choice for determining aflatoxins and is also growing in popularity for their identification. The reasons for selecting HPLC over TLC can be summarized as the ability to analyze for a wide variety of compounds, including compounds that are easily degraded by heat, light or air, the ease of adaptation to confirmatory procedures, the potential for automation and the dramatic improvement in instrumentation, including the development of increasingly sensitive fluorescence and electrochemical detectors and short, high-resolution, reversed-phase columns. 相似文献