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1.
The reversed‐phase mode of single drop microextraction has been used as a preparation method for the extraction of some phenolic antioxidants from edible oil samples. Butylated hydroxyl anisole, tert‐butylhydroquinone and butylated hydroxytoluene were employed as target compounds for this study. High‐performance liquid chromatography followed by fluorescence detection was applied for final determination of target compounds. The most interesting feature of this study is the application of a disposable insulin syringe with some modification for microextraction procedure that efficiently improved the volume and stability of the solvent microdrop. Different parameters such as the type and volume of solvent, sample stirring rate, extraction temperature, and time were investigated and optimized. Analytical performances of the method were evaluated under optimized conditions. Under the optimal conditions, relative standard deviations were between 4.4 and 10.2%. Linear dynamic ranges were 20–10 000 to 2–1000 μg/g (depending on the analytes). Detection limits were 5–670 ng/g. Finally, the proposed method was successfully used for quantification of the antioxidants in some edible oil samples prepared from market. Relative recoveries were achieved from 88 to 111%. The proposed method had a simplicity of operation, low cost, and successful application for real samples.  相似文献   

2.
In this article, we proposed very simple procedures to analyze important phenolic compounds in olive oil samples from different olive varieties. A nonaqueous CE method has been employed. The main phenolic alcohols in virgin olive oil (tyrosol and hydroxytyrosol) and some among the most abundant secoiridoid aglycone derivatives (dialdehydic form of decarboxymethyl elenoic acid linked to hydroxytyrosol, an isomer of oleuropein aglycone and the dialdehydic form of decarboxymethyl elenoic acid linked to tyrosol) were determined by a direct injection into the capillary of the olive oil dissolved in 1‐propanol 1:1 v/v. For the determination of compounds present at lower concentrations, a very simple liquid–liquid extraction method with ethanol has been proposed. The extraction was performed using a relationship 5:1 w/v olive oil/ethanol to achieve the necessary preconcentration of the analytes and the ethanolic extracts were directly injected into the capillary to obtain a very important time reduction. Good recoveries were obtained with both the procedures, using an internal standard. Finally, these procedures were applied to the analysis of these compounds in extra virgin olive oil samples from different varieties of olive.  相似文献   

3.
A new efficient method was developed to detect biotin in Antarctic krill by Vis‐absorbance detection. DMF was used after chloroform pretreatment to extract biotin and two chromogenic methods were developed. The development system consisted of dichloromethane/dimethylcarbinol/methanol/glacial acetic acid (3:3:2:0.015, v/v/v/v). Samples were separated on precoated silica gel GF254 high‐performance TLC plates. Densitometric analysis of biotin was carried out in the absorbance mode at 400 and 530 nm. The biotin content was determined to be 1.0948 ± 0.0097 and 1.1212 ± 0.0155 mg/g in Antarctic krill with the two chromogenic methods, which had no significant difference.  相似文献   

4.
The combined use of a dual‐UV detector, a fluorimetric one and of a multiple electrochemical (EC) detector equipped with a dual electrode, consisting of a conventional size 3 mm diameter glassy carbon electrode (GCE) and of a pair of 30 μm thick carbon microfibers, is proposed for the determination of 15 amino acids, two dipeptides and creatinine. This online coupling of the above detection modes could partially replace amino acid analysis by derivatization methods, since it solves problems concerning the direct detection of selected underivatized amino acids. Additionally, it was proved that the use of multiple‐detection allows positive peak identification in a single chromatographic run, yields more information for free amino acids and solves in some cases the problem of chromatographic resolution. In order to optimize the detection conditions of the underivatized amino acids and related compounds by different detectors, their detection characteristics were determined by adequate preliminary experiments. The electro‐oxidation characteristics of the underivatized compounds of interest were determined by hydrodynamic voltammetry using a flow cell with a macrodisc GCE and by ex‐situ voltammetry using both a GCE of conventional size and a carbon fiber disk microelectrode. Important practical advantages of microfiber and microdisk electrodes with respect to macroelectrodes were demonstrated.  相似文献   

5.
In this study, a simple, rapid, and sensitive method for the determination of nitrite (NO2?) in food samples by high‐performance liquid chromatography with fluorescence detection in acidic conditions had been developed. The derivatization of the nitrite with 2,3‐diaminonaphthalene was performed in acidic conditions to yield the highly fluorescent 2,3‐naphthotriazole, which was directly analyzed by high‐performance liquid chromatography with fluorescence detection without adjusting the solution to alkaline. The analysis column was reversed‐phase C8 column. A constant flow rate of 1.0 mL/min was employed using water/acetonitrile as the mobile phase in isocratic mode (70:30, v/v). Fluorescence was monitored with excitation at 375 nm and emission at 415 nm. The standard calibration curves were linear for nitrite in different matrixes in the concentration range of 0–100 μg/L, and the correlation coefficients ranged from 0.9978 to 0.9998. The limits of detection and quantification were in the ranges of 0.012–0.060 and 0.040–0.20 mg/kg, respectively. The recoveries of nitrite from samples spiked at three different concentrations were 74.0–113.2%, and the relative standard deviations of the recovery results (n = 6) were 1.67–10.8%. The proposed method has good repeatability and is very sensitive and simple. It has been successfully used to determine nitrite in foods.  相似文献   

6.
4,4′‐Diaminostilbene‐2,2′‐disulfonic acid based fluorescent whitening agents (DSD‐FWAs) are prohibited in food‐contact paper and board in many countries. In this work, a reliable high‐performance liquid chromatography method was developed for the simultaneous determination of 11 common DSD‐FWAs in paper material. Sample preparation and extraction as well as chromatographic separation of multicomponent DSD‐FWAs were successfully optimized. DSD‐FWAs in prepared samples were ultrasonically extracted with acetonitrile/water/triethylamine (40:60:1, v/v/v), separated on the C18 column with the mobile phase containing tetrabutylammonium bromide, and then detected by a fluorescence detector. The limits of detection were 0.12–0.24 mg/kg, and the calibration curves showed the linear correlation (R2 ≥ 0.9994) within the range of 8.0–100 ng/mL, which was equivalent to the range of 0.80–10 mg/kg in the sample. The average recoveries and the RSDs were 81–106% and 2–9% at two fortification levels (1.0 and 5.0 mg/kg) in paper bowls, respectively. The successful determination of 11 DSD‐FWAs in food‐contact paper and board obtained from local markets indicated that the newly developed method was rapid, accurate, and highly selective.  相似文献   

7.
We developed a method for the simultaneous quantification of 7‐O‐succinyl macrolactin A and its active metabolite, macrolactin A, in dog plasma. After protein precipitation with acetonitrile including flufenamic acid as an internal standard, 7‐O‐succinyl macrolactin A, macrolactin A, and flufenamic acid were chromatographed on a reverse‐phase C18 analytical column. The mobile phase, consisting of 20 mM acetate buffer and acetonitrile, was eluted using a gradient program at 1 mL/min, and the UV absorbance was measured at 230 nm. The retention times of 7‐O‐succinyl macrolactin A, flufenamic acid, and macrolactin A were 3.4, 4.8, and 6.9 min, respectively. The coefficient of variation in the assay precision for both substances was less than 6%, and the accuracy ranged from 96 to 105%. This method was used to measure the concentrations of 7‐O‐succinyl macrolactin A and macrolactin A in dog plasma following an intravenous administration of a single dose (25 mg/kg) of 7‐O‐succinyl macrolactin A salt.  相似文献   

8.
Intravenous immunoglobulin (IVIg) is increasingly used for the treatment of autoimmune and systemic inflammatory diseases with both licensed and off‐label indications. Recent studies indicated that IVIg‐mediated immunomodulation and anti‐inflammation are closely associated with the IgG sialylation, especially with IgG crystallizable fragment (Fc) sialylation. The sialic acid levels of the IgG molecules and Fc fragments in 12 IVIg preparations from six Chinese manufacturers were evaluated. The Fc fragments were derived from the papain digestion of IVIg, followed by affinity and size exclusion chromatography. The sialic acid levels in Fc fragments and IVIg preparations were determined by high‐performance liquid chromatography with fluorescence detection, after the sialic acid residues were released from the proteins. The results showed that the sialic acid levels in Chinese IVIg preparations ranged from 0.875 (mol/mol IgG) to 1.085 (mol/mol IgG), and the sialic acid levels in Fc fragments were from 0.321 (mol/mol Fc) to 0.361 (mol/mol Fc). Furthermore, the sialic acid levels of IVIg preparations and Fc fragments from different Chinese manufactures were significantly different. These findings will contribute to an increased understanding of Chinese IVIg preparations and the relationship between the sialic acid levels in IVIg preparations and their clinical efficacy in future clinical studies.  相似文献   

9.
Plasma samples were conventionally stored at freezing conditions until the time of detection. Such a technique, when carried out over an extended period, is energy consuming; in addition, preparation and transportation of stored samples is inconvenient. In this study, a freeze‐dried storage and preparation method was proposed to determine the presence of mycophenolic acid (MPA) in plasma. Fresh plasma samples were freeze‐dried using a device, and then stored at ambient temperature. After the stored samples were soaked with methanol spiked with the internal standard, high‐performance liquid chromatography was conducted to detect MPA. The proposed method was demonstrated to be precise and accurate over the linear range of 0.5–50 μg mL−1, with both intra‐ and inter‐day precision being <7% and biases <10%. The freeze‐dried samples were stable at ambient temperature for at least 40 days. This method was also successfully applied to the pharmacokinetic study of MPA in healthy volunteers. Pharmacokinetic parameters, such as maximum plasma concentration, time point of maximum plasma concentration and elimination half‐life, among others, were consistent with the results in the published study. This proposed technique was proved to be simple, reproducible and energy saving. This approach could also simplify the storage and analysis of samples in clinical and scientific drug research.  相似文献   

10.
A simple, fast, and sensitive analytical protocol using fabric‐phase sorptive extraction followed by high performance liquid chromatography with ultraviolet detection has been developed and validated for the extraction of five parabens including methylparaben, ethylparaben, propylparaben, butylparaben, and benzylparaben. In the present work, sol‐gel polyethylene glycol coated fabric‐phase sorptive extraction membrane is used for the preconcentration of parabens (polar) from complex matrices. The use of fabric‐phase sorptive extraction membrane provides a high surface area which offers high sorbent loading, shortened equilibrium time, and overall decrease in the sample preparation time. Various factors affecting the performance of fabric‐phase sorptive extraction, including extraction time, eluting solvent, elution time, and pH of the sample matrix, were optimized. Separation was performed using a mobile phase consisting of water:acetonitrile (63:37; v/v) at an isocratic elution mode at a flow rate of 0.9 mL/min with wavelength at 254 nm. The calibration curves of the target analytes were prepared with good correlation coefficient values (r2 > 0.9955). The limit of detection values range from 0.252 to 0.580 ng/mL. Finally, the method was successfully applied to various cosmetics and personal care product samples such as rose water, deodorant, hair serum, and cream with extraction recoveries ranged between 88 and 122% with relative standard deviation <5%.  相似文献   

11.
Organoleptic properties of flaxseed oil deteriorate during storage due to methionine oxidation in its major cyclolinopeptides. Cyclolinopeptide E was previously identified as being responsible for the manifestation of bitter taste with flaxseed oil ageing. We developed a chromatographic procedure to monitor the oxidation of major cyclic peptides in flaxseed oil. We also used liquid chromatography with mass spectrometry and high‐efficiency core–shell reversed‐phase sorbents to study the separation of cyclolinopeptides in detail. The KinetexTM family of stationary phases (C8, C18, phenyl‐hexyl) was tested, along with the standard porous LunaTM C18(2) media. We found that only the phenyl‐hexyl stationary phase allows for complete resolution of major cyclolinopeptides, thus permitting direct UV monitoring of degree of conversion for cyclolinopeptide B into C and L into E. We also report, for the first time, a significant effect of peak splitting for some methionine S‐oxide (Mso) containing cyclolinopeptides, which most likely appear due to diastereomerization. This results in poor separation efficiency for cyclolinopeptides F, G, and E, and gives baseline resolution of diastereomeric pairs for cyclolinopeptides I and P. Thus, a single oxidation of cyclolinopeptide N yields three distinct chromatographic peaks corresponding to cyclolinopeptide T (cyclo‐MsoLMPFFWV, reported for the first time) and pair of cyclolinopeptide I (cyclo‐MLMsoPFFWV) diastereomers.  相似文献   

12.
In this study, a qualitative and quantitative analysis using high‐performance liquid chromatography coupled to electrospray ionization and quadrupole time‐of‐flight mass spectrometry was performed for the quality control of Bu‐Shen‐Yi‐Qi‐Fang, a traditional Chinese formula used for asthma. Thirty‐four compounds, including flavonoids, isoflavonoids, triterpenoid saponins, and iridoid glycosides were identified or tentatively characterized by comparing their retention times and mass spectra with those of authentic standards or literature data. Sixteen components were considered as the main bioactive constituents of Bu‐Shen‐Yi‐Qi‐Fang and they were chosen as the chemical markers in quantitative analysis, including catalpol, leonuride, calycosin‐7‐O‐β‐d ‐glucoside, hyperoside, acteoside, formononetin‐7‐O‐β‐d ‐glucoside, epimedin A, calycosin, icariin, epimedin B, epimedin C, formononetin, astragaloside IV, astragaloside II, baohuoside‐I, and astragaloside I. The total run time was 20 min. It was found that the calibration curves for all analytes showed good linearity (R2 > 0.99) within the test ranges. The relative standard deviations for intra‐ and inter‐day precisions were below 3.9 and 11.7%, respectively. The accuracy was evaluated by the recovery test within the range of 89.20–110.71% with the relative standard deviation < 4.8%. The sample was stable for at least 48 h at 4°C. The results showed that the new approach was effective for the quality control of Bu‐Shen‐Yi‐Qi‐Fang.  相似文献   

13.
A selective, sensitive and rapid high‐performance liquid chromatography method with post‐column hydrolysis and fluorescence detection was developed for the simultaneous quantification of acetylsalicylic acid and its metabolite salicylic acid in human plasma. Following the addition of 2‐hydroxy‐3‐methoxybenzoic acid as internal standard and simple protein precipitation with acetonitrile, the analytes were separated on a ProntoSIL 120 C18 ace‐EPS column (150 × 2 mm, 3 µm) protected by a C8 guard column (5 µm). The mobile phase, 10 mm formic acid in water (pH 2.9) and acetonitrile (70:30, v/v), was used at a flow rate of 0.35 mL/min. After on‐line post‐column hydrolysis of acetylsalicylic acid (ASA) to salicylic acid (SA) by addition of alkaline solution, the analytes were measured at 290 nm (λex) and 400 nm (λem). The method was linear in the concentration ranges between 0.05 and 20 ng/μL for both ASA and SA with a lower limit of quantification of 25 pg/μL for SA and 50 pg/μL for ASA. The limit of detection was 15 pg/μL for SA and 32.5 pg/μL for ASA. The analysis of ASA and SA can be carried out within 8 min; therefore this method is suitable for measuring plasma concentrations of salicylates in clinical routine. Copyright © 2012 John Wiley & Sons, Ltd.  相似文献   

14.
How to determine the multipesticide residues in vegetables is an important problem. In this study, a new molecularly imprinted polymer was synthesized using O,O‐dimethyl thiophosphoryl chloride, an intermediate for the manufacture of organophosphorous pesticides, as the template. Characterization test indicated that the synthesized polymer exhibited good recognition and selectivity for dichlorvos, methamidophos, acephate, folimat, monocrotophos, parathion‐methyl, phosphamidon, and malathion. A molecularly imprinted SPE coupled to GC for simultaneous separation and determination of eight organophosphorous pesticides residues was developed. Under optimal conditions, the linear range of this method was 0.001–10.0 mg/L. The LOD of this method was in the range of 0.13–0.90 μg/kg. With a flow rate of 2.5 mL/min for loading 100 mL, the enrichment factor in the range of 25–480 for the eight organophosphorous pesticides was obtained. The RSD of the eight organophosphorous pesticides based on five replicates was from 1.50 to 4.09%. The accuracy of the proposed method was evaluated by recovery measurements on spiked samples, and good recovery rates ranging from 80.11 to 97.70% were achieved. Moreover, this method was evaluated for the quantitative detection of eight organophosphorous pesticide residues in leek and pakchoi samples.  相似文献   

15.
Acrolein is a major unsaturated aldehyde that is generated during the lipid peroxidation process. The measurement of acrolein in biological samples should be useful to estimate the degree of lipid peroxidation and to evaluate the effect of hazardous properties of acrolein on human health. In this study, a highly sensitive and selective high‐performance liquid chromatography with fluorescence detection method was developed for the determination of acrolein in human serum. The proposed method involves the pre‐column fluorogenic derivatization of acrolein with 1,2‐diamino‐4,5‐dimethoxybenzene (DDB) as a reagent. The fluorescent derivative of acrolein could be detected clearly without any interfering reagent blank peaks because DDB does not have intrinsic fluorescence itself, and the detection limit was 10 nM (signal‐to‐noise ratio = 3). The proposed method could selectively detect acrolein in human serum with a simple protein precipitation treatment. Copyright © 2015 John Wiley & Sons, Ltd.  相似文献   

16.
Benzotriazole ultra‐violet stabilisers are compounds widely used in personal care products, which can reach the environment after passing through wastewater treatment plants. In this work, we develop a novel method to evaluate the presence of seven compounds in marine sediments and sewage sludges using microwave‐assisted extraction followed by a clean‐up step based in on‐line solid phase extraction coupled to ultra‐high‐performance liquid chromatography with MS/MS detection. This method allows for fast and efficient extraction from the solid matrix, subsequent automatic on‐line purification and preconcentration, and analysis. For the optimised method, LOD were from 53.3 to 146 ng/kg and LOQ were in the range of 176–486 ng/kg. The method was validated for different environmental solid samples with satisfactory recoveries and relative standard deviations, between 46.1 and 83.9 and 7.8 and 15.5% (sludges) and 50.1 and 87.1% and 8.83 and 16.3% (sediments), respectively. Finally, the studied analytes were quantified in concentrations between 0.18 and 24.0 ng/g in real samples of marine sediments and sewage sludges from Gran Canaria Island (Spain).  相似文献   

17.
A method for tryptophan analysis in bee pollen and royal jelly was developed using HPLC with fluorescence detection. To determine the free tryptophan in bee pollen and royal jelly, ultrasonic extraction was performed using water (pH 6.3)–acetonitrile (10:1, v/v) as extraction solvent. While determining the total tryptophan in these bee products, the method involves alkaline hydrolysis of the proteins with 4 mol/L sodium hydroxide at 110°C for 20 h under anaerobic conditions. The operating conditions for the HPLC analysis were: Symmetry C18 column (4.6 × 250 mm, 5 µm), 0.1% trifluoroacetic acid–methanol (75:25, v/v) as the mobile phase at a flow rate of 1.0 mL/min at 30°C. The fluorescence detector was operated at an excitation wavelength of 280 nm and an emission wavelength of 340 nm. A linear response (r> 0.9998) was obtained in the range 0.0625–5.0 µg/mL. The method was successfully applied to the determination of the free and total tryptophan contents in bee pollens, which were 0.069 ± 0.003 and 2.693 ± 0.476 mg/g, respectively, while only the total tryptophan was detected in royal jelly, with a content of 1.743 ± 0.066 mg/g. Copyright © 2009 John Wiley & Sons, Ltd.  相似文献   

18.
Solid‐phase extraction coupled with dispersive liquid–liquid microextraction was developed as an ultra‐preconcentration method for the determination of four organophosphorus pesticides (isocarbophos, parathion‐methyl, triazophos and fenitrothion) in water samples. The analytes considered in this study were rapidly extracted and concentrated from large volumes of aqueous solutions (100 mL) by solid‐phase extraction coupled with dispersive liquid–liquid microextraction and then analyzed using high performance liquid chromatography. Experimental variables including type and volume of elution solvent, volume and flow rate of sample solution, salt concentration, type and volume of extraction solvent and sample solution pH were investigated for the solid‐phase extraction coupled with dispersive liquid–liquid microextraction with these analytes, and the best results were obtained using methanol as eluent and ethylene chloride as extraction solvent. Under the optimal conditions, an exhaustive extraction for four analytes (recoveries >86.9%) and high enrichment factors were attained. The limits of detection were between 0.021 and 0.15 μg/L. The relative standard deviations for 0.5 μg/L of the pesticides in water were in the range of 1.9–6.8% (n = 5). The proposed strategy offered the advantages of simple operation, high enrichment factor and sensitivity and was successfully applied to the determination of four organophosphorus pesticides in water samples.  相似文献   

19.
UV filters, contained in sunscreens and other cosmetic products, as well as in some plastics and industrial products, are nowadays considered contaminants of emerging concern because their widespread and increasing use has lead to their presence in the environment. Furthermore, some UV filters are suspected to have endocrine disruption activity. In the present work, we developed an analytical method based on liquid chromatography with tandem mass spectrometry for the determination of UV filters in tap and lake waters. Sixteen UV filters were extracted from water samples by solid‐phase extraction employing graphitized carbon black as adsorbent material. Handling 200 mL of water sample, satisfactory recoveries were obtained for almost all the analytes. The limits of detection and quantification of the method were comparable to those reported in other works, and ranged between 0.7–3.5 and 1.9–11.8 ng/L, respectively; however in our case the number of investigated compounds was larger. The major encountered problem in method development was to identify the background contamination sources and reduce their contribution. UV filters were not detected in tap water samples, whereas the analyses conducted on samples collected from three different lakes showed that the swimming areas are most subject to UV filter contamination.  相似文献   

20.
Despite the strong antihepatotoxic, antioxidant, and antitumor properties of lignans from Schisandra chinensis, their applications in new drug development, bioscience and functional foods, etc. are limited because of their low abundance and complex coextractions. In this study, a magnetic separation method has been developed based on polyethylenimine‐modified magnetic nanoparticles to rapidly and effectively separate and purify the lignans from S. chinensis crude extracts through cation–π interaction and electrostatic adsorption. The magnetic nanoparticles were characterized by transmission electron microscopy, vibrating sample magnetometry, Fourier transform infrared spectroscopy, and X‐ray diffraction. Polyethylenimine‐modified magnetic nanoparticles showed a spherical‐shaped morphology and the average size was about 10 nm with superparamagnetism. Under the pH 7.4, polyethylenimine modified magnetic nanoparticles can remove a lot of coextracts. The range of detection limits and quantification limits was 0.27–0.34 and 0.89–1.13 ng/mL, respectively. Compared with other common methods, the magnetic separation method proposed in this study is much simpler and more effective through both strong cation–π interaction and electrostatic interaction.  相似文献   

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