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Supramolecular solvent-based microextraction of Sudan dyes in chilli-containing foodstuffs prior to their liquid chromatography-photodiode array determination

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FOOD CHEMISTRY 2010年第3期121卷 763-769页

作者： Jose Lopez-Jimenez, Francisco Rubio, Soledad Perez-Bendito, Dolores Univ Cordoba Dept Analyt Chem E-14071 Cordoba Spain

A supramolecular solvent made up of reverse micelles of decanoic acid was proposed for the simple and rapid extraction of Sudan I, II, III and IV from chilli-containing foodstuffs. The procedure involved the extraction of minute quantities (0.5-1 g) of homogenised food sample with an aqueous solution containing 10% THF and 200 mg of decanoic acid, conditions under which the supramolecular solvent (around 330 mu L) formed in situ and instantaneously. The overall sample treatment took about 30 min and several samples could be simultaneously treated using conventional lab equipment. No clean-up or solvent evaporation were required before determination of Sudan dyes by liquid chromatography and photometric detection. Extractions were independent of salt addition (up to 1 M), the temperature (up to 60 degrees C) and the pH (below 4) rendering the method robust. The detection limits of the method were 4.2, 2.7, 6.5 and 7.4 mu g kg(-1) for Sudan I, II, III and IV, respectively. Recoveries obtained by applying this approach to the analysis of six chilli-containing sauces fortified with Sudan dyes at the mu g kg(-1) level were in the interval 86-108% with relative standard deviations between 2% and 7%. (C) 2010 Elsevier Ltd. All rights reserved.

关键词： Supramolecular solvent Reverse micelles Microextraction Sudan dyes Chilli-containing foodstuffs Liquid chromatography diode array detection

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Elevated Circulating LDL Phenol Levels in Men Who Consumed Virgin Rather Than Refined Olive Oil Are Associated with Less Oxidation of Plasma LDL

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JOURNAL OF NUTRITION 2010年第3期140卷 501-508页

作者： de la Torre-Carbot, Karina Chavez-Servin, Jorge L. Jauregui, Olga Castellote, Ana I. Lamuela-Raventos, Rosa M. Nurmi, Tarja Poulsen, Henrik E. Gaddi, Antonio V. Kaikkonen, Jari Zunft, Hans-Franz Kiesewetter, Holger Fito, Montserrat Covas, Maria-Isabel Carmen Lopez-Sabater, M. Univ Barcelona Fac Pharm Dept Nutr & Food Sci Reference Ctr Food Technol E-08028 Barcelona Spain CIBER Epidemiol & Salud Publ Barcelona 08020 Spain Univ Barcelona Sci & Tech Serv E-08028 Barcelona Spain Univ Kuopio Publ Hlth Res Inst FIN-70211 Kuopio Finland Univ Copenhagen Hosp Rigshosp Dept Clin Pharmacol DK-2200 Copenhagen Denmark Univ Bologna GC Descovich Atherosclerosis & Metab Dis Res Unit I-40138 Bologna Italy Oy Jurilab Kuopio 70210 Finland German Inst Human Nutr D-14558 Potsdam Germany Charite D-10117 Berlin Germany Hosp Mar Inst Municipal Invest Med Lipids & Cardiovasc Epidemiol Unit Barcelona 08003 Spain

In human LDL, the bioactivity of olive oil phenols is determined by the in vivo disposition of the biological metabolites of these compounds. Here, we examined how the ingestion of 2 similar olive oils affected the content of the metabolic forms of olive oil phenols in LDL in men. The oils differed in phenol concentrations as follows: high (629 mg/L) for virgin olive oil (VOO) and null (0 mg/L) for refined olive oil (ROO). The study population consisted of a subsample from the EUROLIVE study and a randomized controlled, crossover design was used. Intervention periods lasted 3 wk and were preceded by a 2-wk washout period: The levels of LDL hydroxytyrosol monosulfate and homovanillic acid sulfate, but not of tyrosol sulfate, increased after VOO ingestion (P < 0.05), whereas the concentrations of circulating oxidation markers, including oxidized LDL (oxLDL), conjugated dienes, and hydroxy fatty acids, decreased (P < 0.05). The levels of LDL phenols and oxidation markers were not affected by ROO consumption. The relative increase in the 3 LDL phenols was greater when men consumed VOO than when they consumed ROO (P < 0.05), as was the relative decrease in plasma oxLDL (P = 0.001) and hydroxy fatty acids (P < 0.001). Plasma oxLDL concentrations were negatively correlated with the LDL phenol levels (r = -0.296;P = 0.013). Phenols in LDL were not associated with other oxidation markers. In summary, the phenol concentration of olive oil modulates the phenolic metabolite content in LDL after sustained, daily consumption. The inverse relationship of these metabolites with the degree of LDL oxidation supports the in vivo antioxidant role of olive oil phenolics compounds. J. Nutr. 140: 501-508, 2010.

关键词： DAD diode array detection MS/MS tandem MS oxLDL oxidized LDL ROO refined olive oil VOO virgin olive oil

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Dispersive liquid-liquid microextraction combined with high performance liquid chromatography-DAD detection for the determination of sulfonylurea herbicides in water samples

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INTERNATIONAL JOURNAL OF ENVIRONMENTAL ANALYTICAL CHEMISTRY 2010年第11期90卷 891-902页

作者： Wu, Qiu Hua Li, Yun Peng Li, Chao Wu, Chun Xia Liu, Zhi Mei Hou, Yu Xuan Wang, Zhi Agr Univ Hebei Coll Sci Key Lab Bioinorgan Chem Baoding 071001 Peoples R China Agr Univ Hebei Coll Life Sci Baoding 071001 Peoples R China

A new method for the determination of four sulfonylurea herbicides (metsulfuron-methyl, chlorsulfuron, bensulfuron-methyl and chlorimuron-ethyl) in water samples was developed by dispersive liquid-liquid microextraction coupled with high performance liquid chromatography-diode array detector. Parameters that affect the extraction efficiency, such as the kind and volume of the extraction and disperser solvent, extraction time and salt addition, were investigated and optimised. Under the optimum conditions, the enrichment factors were in the range between 102 and 216. The linearity of the method was obtained in the range of 1.0-100 ng mL-1 with the correlation coefficients (r) ranging from 0.9982 to 0.9995. The method detection limits were 0.2-0.3 ng mL-1. The proposed method has been successfully applied to the analysis of target sulfonylurea herbicides in river, stream and well water samples with satisfactory results.

关键词： sulfonylurea herbicides high performance liquid chromatography diode array detection dispersive liquid-liquid microextraction water samples

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Identification and Determination of the Major Constituents in the Traditional Uighur Medicinal Plant Saussurea involucrata by LC-DAD-MS

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CHROMATOGRAPHIA 2009年第5-6期69卷 537-542页

作者： Yi, Tao Chen, Hu-Biao Zhao, Zhong-Zhen Jiang, Zhi-Hong Cai, Shao-Qing Wang, Tian-Min Hong Kong Baptist Univ Sch Chinese Med Hong Kong Hong Kong Peoples R China Peking Univ Hlth Sci Ctr Sch Pharmaceut Sci State Key Lab Nat & Biomimet Drugs Beijing 100083 Peoples R China

A liquid chromatography coupled with diode array detector and electrospray ionization mass spectrometry method was developed for the simultaneous analysis of the major constituents in Saussurea involucrata (SI). A comprehensive validation of the developed method was conducted, and the unique properties of the present method were confirmed by analyzing 11 SI samples. Seventeen compounds including phenolic acids, flavonoids, and lignanoids were identified by online ESI-MS and by comparison with known data in the literature and standard compounds;of these, eight were simultaneously quantified by LC-DAD. All linear regressions were acquired with R (2) > 0.99, and the limits of detection ranged from 0.85 to 3.03 ng. Repeatability was evaluated by intra- and inter-day assays;the relative standard deviation (RSD) value was within 4.95%. Recovery studies for the quantified compounds were found to be within the range 97.31-101.17% with an RSD of less than 2.18%. Overall, the present hyphenation procedure is highly efficient and reliable, and hence suitable for qualitative and quantitative analysis of a large number of samples.

关键词： Column liquid chromatography diode array detection Electrospray ionisation mass spectrometry Pharmaceutical analysis Ethnopharmacy Saussurea involucrata

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Fingerprint Comparison Between Gegen Qinlian Preparations of Three Different Pharmaceutical Forms Including Decoction, Dispensing Granule and Pill

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CHROMATOGRAPHIA 2009年第1-2期69卷 123-127页

作者： Chen, Lihong Liu, Jining Wang, Qiang Chen, Jiahui China Pharmaceut Univ Dept Chinese Meteria Med Anal Nanjing 210009 Peoples R China Nanjing Univ Chinese Med Jiangsu Key Lab TCM Formulae Res Nanjing 210046 Peoples R China SEPA Nanjing Inst Environm Sci Nanjing 210042 Peoples R China Simcere Pharmaceut Co Ltd Nanjing 210042 Peoples R China

Gegen Qinlian decoction, a favorite composite formula of Chinese medicine, has been made into various formulations. Pill and dispensing granule are currently very popular dosage forms for oral application. To ensure consistent therapeutic effects, fingerprint comparison between Gegen Qinlian preparations of three pharmaceutical forms including decoction, dispensing granule and pill is carried out to investigate influence of dosage forms on patterns of components in the composite formula. The fingerprint analysis demonstrates that, in relationship to baicalin with its area set to 1, most of the area ratios of 20 common peaks in decoction and dispensing granule vary little except the area ratio of puerarin (0.805 in decoction vs. 0.593 in dispensing granule), berberine (0.400 in dispensing granule vs. 0.283 in decoction) and the peak of baicalein, which originally observed in dispensing granule decrease substantially in decoction. However, in pills the area ratios of the common peaks are significantly different from those in dispensing granule except for peak 29. The inconsistencies among patterns of components in three types of Gegen Qinlian preparations, especially between dispensing granule and pill, may result in different pharmacological effects.

关键词： Column liquid chromatography diode array detection Fingerprint comparison Gegen Qinlian preparations

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Optimization of CDTE Quantum Dots Synthesis Using Capillary Zone Electrophoresis

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CURRENT NANOSCIENCE 2009年第2期5卷 154-159页

作者： Clarot, Igor Wolpert, Cecile Morosini, Vincent Schneider, Raphael Balan, Lavinia Diez, Laurent Leroy, Pierre Nancy Univ Fac Pharm CNRS Grp Etud Vecteurs Supramol MedicametUMR 7565 F-54001 Nancy France Nancy Univ Fac Pharm Lab Chim Analyt & Bioanal Medicament F-54001 Nancy France Nancy Univ Fac Pharm CNRS Lab Chim Phys & Microbiol Environm F-54001 Nancy France Nancy Univ CNRS DCPR F-54001 Nancy France Univ Haute Alsace ENSCMu CNRS Dept Photochim GenUMR 7525 F-68093 Mulhouse France

Water-soluble, thiol protected cadmium telluride CdTe quantum dots (QDs) exhibit size dependent excitation/emission wavelength tunability. The heating period ensuring the growth of CdTe nanocrystals capped with thioglycolic acid (CdTe@TGA) in aqueous solution is critical to reach a required/desirable diameter. Thus, reaction medium was monitored using a capillary zone electrophoresis (CZE) technique in order to select an appropriate heating time. QDs migrate as anionic species in a borate buffer pH 8.5 used as background electrolyte and they were separated according to their size (larger ones have shorter migration times), as confirmed by measuring their maximum wavelength of absorption, with on-line diode array detection. A relationship between electrophoretic mobilities and lambda(max) was tentatively proposed. Efficiency of the purification process of crude QDs using multiple step alcohol precipitation was also confirmed with the developed CZE technique.

关键词： Quantum dots synthesis size-selective precipitation capillary zone electrophoresis diode array detection size-dependent migration

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Simultaneous Determination of Antibiotics in Anti-Acne Cosmetics by Rapid LC with DAD

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CHROMATOGRAPHIA 2009年第11-12期69卷 1221-1226页

作者： Jin, Wei Yang, Yong-Jian Wang, Wei-Yu Ye, Jian-Nong E China Normal Univ Dept Chem Shanghai 200062 Peoples R China Shanghai Inst Food & Drug Control Shanghai 201203 Peoples R China

A suitable method that allows, for the first time, the simultaneous determination of nine antibiotics which may help the therapy of acne vulgaris by rapid liquid chromatography with diode array detection in 7 min is presented in this work. An SB RP18 (50 x 4.6 mm;1.8 mu m particle size) column was used with the mobile phase consisting of a mixture of 0.1 mol L-1 potassium clihydrogen phosphate (pH 2.5) and acetonitrile at the gradient elution program. The correlation coefficients were all above 0.9999 in the linear range between 4-100 mu g mL(-1), the average spiked recoveries (n = 6) were 92.2-103.2% with RSD ranging from 0.04 to 4.5% depending on the target analytes. The method detection limits were in the range of 0.02-0.2 mu g mL(-1) in anti-acne cosmetics. The analysis of real cosmetic preparations demonstrated the fitness for the whole analytical procedure. The proposed method appeared therefore as a sound alternative for official testing method, which could overcome the general problems of time consuming, lack of the specificity and precision difficulty.

关键词： Column liquid chromatography diode array detection Anti-acne cosmetics Antibiotics

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Fingerprint Analysis of Euonymus alatus (Thuhb) siebold by LC-DAD and LC-ESI-MS

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CHROMATOGRAPHIA 2009年第5-6期69卷 429-436页

作者： Zhao, Zhan-Yi Dong, Lu-Lu Lin, Feng Harbin Med Univ Coll Pharm Harbin 150086 Peoples R China Post Doctor Working Stn Yuanda Grp Harbin 150086 Peoples R China

A liquid chromatography coupled with photodiode array detection and electrospray ionization tandem mass spectrometry method was first developed for a chemical fingerprint analysis of Euonymus alatus (Thuhb) siebold (EAS) and rapid identification of major compounds in the fingerprints. Fingerprint profiles were found to be consistent for the herbs acquired from different locations, but the relative abundance of peaks was varied. Twelve peaks were chosen as the common peaks. Quercetin and rutin were detected by comparing the retention times, MS and UV spectra with the standards. The relative retention time and relative peak area of the 12 peaks in the fingerprint were calculated by setting the quercetin as the reference peak. The experimental data were used for similarity calculation and hierarchical clustering analysis. By comparing the UV and MS spectra data with those of the authentic standards and literature, five main peaks in the fingerprints were identified. Finally, five medicinal portions of the herb (leaf, fruit, stem, pterygium and root) were also analyzed by this method. It was found that there were similar chemical components in different parts of this herb but the contents were very different. The developed fingerprint assay was specific and could be readily utilized for comprehensive evaluation of EAS, as well as to distinguish different medicinal portions.

关键词： Column liquid chromatography diode array detection Electrospray ionization tandem mass spectrometry Fingerprint Quality control Euonymus alatus (Thuhb) siebold

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Quantitative and qualitative control of cytotoxic preparations by HPLC-UV in a centralized parenteral preparations unit

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JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS 2009年第5期49卷 1213-1220页

作者： Delmas, A. Gordien, J. B. Bernadou, J. M. Roudaut, M. Gresser, A. Malki, L. Saux, M. C. Breilh, D. CHU Bordeaux Pharm Hop Haut Leveque Pessac France Univ Bordeaux 2 Lab Pharmacocinet Clin EA2968 Bordeaux France Univ Bordeaux 2 Pharm Clin Grp PK PD Bordeaux France

The constantly growing incidence of cancer and long-term treatment are leading to an increasing number of cytotoxic preparations in hospital pharmacies. Security and quality standards of cytotoxic preparations are essential to assure treatment efficiency and limit iatrogenic toxicity. In order to secure the process of cytotoxic preparations;we decided to install a quantitative and qualitative High Performance Liquid Chromatography (HPLC) control of cytotoxic preparations carried inside our pharmacotechnic unit. A 100 mu l sample of each preparation was assayed by HPLC with ultraviolet/visible-diode array detection, which enabled the identification of all cytotoxic agents thanks to their characteristic UV spectra. We developed rapid and specific HPLC assays that determined qualitatively and quantitatively the presence of 21 different cytotoxic agents in less than 3.5 min. A fifteen per cent tolerance from the theoretical concentration was chosen in agreement with preparation and dosage bias, and a first period control of more than 4400 preparations revealed that around 7.7% preparations did not conform. The main objective of these controls was to avoid the administration of defective chemotherapies to patients and finally to use their results to identify error factors;as a result we will take corrective measures in order to reduce error frequency. (C) 2009 Elsevier B.V. All rights reserved.

关键词： Cytotoxic Control HPLC-UV Quality assurance diode array detection

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Novel method for the determination of five carbamate pesticides in water samples by dispersive liquid-liquid microextraction combined with high performance liquid chromatography

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Chinese Chemical Letters 2009年第2期20卷 213-216页

作者： Zhi Mei Liu Xiao Huan Zang Wei Hua Liu Chun Wang Zhi Wang Key Laboratory of Bioinorganic Chemistry College of Sciences Agricultural University of Hebei Baoding 071001 China

A novel method for the determination of five carbamate pesticides （metolcarb, carbofuran, carbaryl, isoprocard and diethofencard） in water samples was developed by dispersive liquid-liquid microextraction （DLLME） coupled with high performance liquid chromatography-diode array detector （HPLC-DAD）. Some experimental parameters that influence the extraction efficiency were studied and optimized to obtain the best extraction results. Under the optimum conditions for the method, the calibration curve was linear in the concentration range from 5 to 1000 ng mL^-1 for all the five carbamate pesticides, with the correlation coefficients （r^2） varying from 0.9984 to 0.9994. Good enrichment factors were achieved ranging from 80 to 177- fold, depending on the compound. The limits of detection （LODs）（S/N = 3） were ranged from 0.1 to 0.5 ng mL^-1. The method has been successfully applied to the analysis of the pesticide residues in environmental water samples.

关键词： Carbamate pesticides High performance liquid chromatography diode array detection Dispersive liquid-liquid microextraction Water samples

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