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1.
Nanotechnology ; 32(33)2021 May 25.
Artigo em Inglês | MEDLINE | ID: mdl-33957607

RESUMO

Highly efficient, all-solution processed inverted quantum dot light-emitting diodes (QLEDs) are demonstrated by employing 1,3,5-tri(m-pyrid-3-yl-phenyl)benzene (TmPyPB) layer as electron blocking layer. Electron injection from ZnO electron transport layer to quantum dots (QDs) emission layer (EML) can be adjusted by thickness of TmPyPB layer, enabling the balanced charge carriers in QDs EML. With optimal thickness of this TmPyPB adjuster, 59.7% increment in the device current efficiency (from 8.2 to 13.1 cd A-1) and 46.2% improvement in the maximum luminance (from 31916 to 46674 cd m-2) are achieved, compared with those of the control QLED which has double hole transport layer structure. On the other hand, we find luminescence quenching process, which often happens at the interface of ZnO nanoparticles and QDs, is not obvious in our QLEDs, in which the ZnO layer is fabricated in precursor method, and this conclusion is verified through Time Resolution Photoluminescence test. In a word, this strategy provides a direction for optimizing charge carrier balance in all-solution processed inverted QLED.

2.
Nanotechnology ; 32(32)2021 May 17.
Artigo em Inglês | MEDLINE | ID: mdl-33910184

RESUMO

The photostability issue of CsPbX3(X = Cl, Br, I) quantum dots (QDs) is one of the key origins for the degradation of their luminescence performance, which hinders their application in lighting and displays. Herein, we report a new method combining doping and ligand engineering, which effectively improves the photostability of CsPbBr3QDs and the performance of QD light-emitting diodes (QLEDs). In this method, ZnBr2is doped into CsPbBr3QDs to reduce surface anion defects; didodecyldimethyl ammonium bromide (DDAB) and tetraoctylammonium bromide (TOAB) hybrid ligands, which have strong adsorption with QDs, are employed to protect the surface and enhance the conductivity of QD layer in QLEDs. The photoluminescence (PL) and transmission electron microscopy measurements prove the effectively improved photostability of CsPbX3QDs. Moreover, reduced defects and improved conductivity by doping and hybrid ligands treatment also enable the improved electroluminescence performance of CsPbX3QDs. The maximum luminance and external quantum efficiency of the QLED with optimized CsPbX3QDs are 3518.9 cd m-2and 5.07%, which are 3.6 and 2.1 times than that of the control device, respectively. Combining doping and hybrid ligands makes perovskite QDs have an extremely promising prospect in future applications of high-definition displays, high-quality lighting, as well as solar cells.

3.
Guang Pu Xue Yu Guang Pu Fen Xi ; 34(2): 316-21, 2014 Feb.
Artigo em Zh | MEDLINE | ID: mdl-24822392

RESUMO

In this paper, the blue light properties of LED illumination devices have been investigated. Against the status quo of China's LED lighting, we measured the spectrum component of LED lamps and analyzed the photobiological safety under the current domestic and international standards GB/T 20145-2006/CIE S009/E: 2002 and IEC62471: 2006 standards as well as CTL-0744_2009-laser resolution, which provides the reference to the manufacture of LED lighting lamps as well as related safety standards and laws. If the radiance intensity of blue light in LED is lower than 100 W x m(-2) x Sr(-1), there is no harm to human eyes. LEDs will not cause harm to human eyes under normal use, but we should pay attention to the protection of special populations (children), and make sure that they avoid looking at a light source for a long time. The research has found that the blue-rich lamps can affect the human rule of work and rest, and therefore, the LED lamps with color temperature below 4 000 K and color rendering index of 80 are suitable for indoor use. At the same time, the lamps with different parameters should be selected according to the different distances.


Assuntos
Luz , Iluminação/efeitos adversos , Iluminação/instrumentação , Cor , Humanos
4.
Food Funct ; 12(21): 10423-10431, 2021 Nov 01.
Artigo em Inglês | MEDLINE | ID: mdl-34596192

RESUMO

Yeast mannans from Saccharomyces cerevisiae (123.2 kDa, 40.5 kDa and 21.3 kDa) were prepared. The scavenging abilities of Fe2+, OH˙, and O2˙- and protective capacities against lipid peroxidation and oxidative DNA damage increased with the reduction of the molecular weights of yeast mannans. The highest scavenging abilities of Fe2+, OH˙ and O2˙- (25.32%, 70.8%, and 61.5%) were observed with YM-90, and it showed an anti-lipid peroxidation capacity of 65.82%, which was much stronger than that of vitamin C (VC), with a thiobarbituric acid-reactive substance (TBARS) inhibition rate of 80.41%. However, the highest DPPH scavenging rate (88.7%) was exhibited by YM-30. In addition, the growth-promoting effect of yeast mannans on Lactobacillus strains was further confirmed, and a 54.2% increment of Lactobacillus plantarum ZWR5 cell viability was achieved by YM-90. The results indicated the potential industrial applications of this yeast mannan technology in therapeutic and nutraceutical production.


Assuntos
Antioxidantes/metabolismo , Lactobacillus/crescimento & desenvolvimento , Lactobacillus/metabolismo , Mananas/metabolismo , Saccharomyces cerevisiae/metabolismo , Sequestradores de Radicais Livres/metabolismo , Peroxidação de Lipídeos/efeitos dos fármacos , Peso Molecular , Estresse Oxidativo/efeitos dos fármacos
5.
ACS Appl Mater Interfaces ; 12(1): 1539-1548, 2020 Jan 08.
Artigo em Inglês | MEDLINE | ID: mdl-31834777

RESUMO

Silica encapsulation effectively elevates the resistance of quantum dots (QDs) against water and oxygen. However, QDs-SiO2 composites present low thermal conductivity and strong thermal accumulation, leading to considerable fluorescence quenching of QDs in optoelectronic devices at high power. Here, a sandwich structural QDs-SiO2-BN nanoplate assembly material (QDs-SiO2-BNAs) is developed to reduce the thermal quenching and enhance the stability of QDs in LEDs. The QDs-SiO2-BNAs is fabricated by embedding QDs-SiO2 into the interlayer of layer-by-layer assembled BN nanoplates, and the BN nanoplates are pretreated by SiO2 encapsulation to strengthen the interaction with QDs-SiO2. This assembly structure endows the QDs with fast heat dissipation and double surface protection against air. The medium power QDs-converted LEDs (QD-LEDs) fabricated by direct on-chip packaging of the QDs-SiO2-BNAs gain 44.2 °C temperature reduction at 0.5 W in comparison with conventional QD-LEDs. After aging, the resulting QD-LEDs present degradation of only 1.2% under sustained driving for 250 h. The QD-LEDs also pass the 1 week reliability test at 85 °C/85% RH with <±0.01 shift of the color coordinates, demonstrating the profound potential of the QDs-SiO2-BNAs in LED lighting and display applications.

6.
Nanomaterials (Basel) ; 10(2)2020 Feb 12.
Artigo em Inglês | MEDLINE | ID: mdl-32059468

RESUMO

CdSe/CdS core-shell quantum rods (QRs) are a promising prospect in optoelectronic applications but usually have a relatively low quantum efficiency and stability. Here, we report on an efficient and stable CdSe/CdS/ZnS QRs-in-matrix assembly (QRAs) by growing and embedding CdSe/CdS QRs in ZnS matrices. Structural characterizations show that the CdSe/CdS QRs are encapsulated and interconnected by ZnS in the QRAs structure. The stable ZnS encapsulation renders the CdSe/CdS QRs high quantum efficiency (QE) up to 85%. The QRAs also present high photo- and thermal-stability and can preserve 93% of the initial QE at 100 °C. The QRAs powder presents a light degradation of only 2% under continuous excitation for 100 h, displaying profound potential in optoelectronic applications. White light-emitting diodes (WLEDs) are fabricated by packaging the QRAs powder as phosphor on top of blue GaN chip. The WLED shows high optical performance and light quality.

7.
Anal Bioanal Chem ; 395(7): 2359-70, 2009 Dec.
Artigo em Inglês | MEDLINE | ID: mdl-19784638

RESUMO

A confirmatory and quantitative method based on liquid chromatography-electrospray ionization tandem mass spectrometry (LC-ESI/MS/MS) has been developed for simultaneous determination of seven photoinitiator residues: benzophenone, (1-hydroxycyclohexyl)phenylketone (Irgacure 184), isopropylthioxanthone (ITX), 2-ethylhexyl-(4-dimethylamino)benzoate (EHA or EHDAB), 2-methyl-1-[4-(methylthio)phenyl]-2-(4-morpholinyl)-1-propanone (Irgacure 907), (2,4,6-trimethylbenzoyl)diphenylphosphine oxide (TPO) and 2-benzyl-2-(dimethylamino)-1-(4-morpholinophenyl)-1-butanone (Irgacure 369) in packaged milk and related packaging materials. Residues of photoinitiators were extracted from milk using acetonitrile, and further enriched and purified on HLB solid-phase extraction cartridges prior to being analyzed by LC-ESI/MS/MS with selected reaction monitoring mode, while photoinitiators in packaging materials were extracted using the same solvent. Satisfactory recovery (from 80 to 111%), intra- and inter-day precision (below 12%), and low limits of quantification (from 0.1 to 5.0 microg kg(-1)) were evaluated from spiked samples at three concentration levels (5.0, 10.0 and 25.0 microg kg(-1) for Irgacure 184 and 2.5, 5.0 and 25.0 microg kg(-1) for others). These excellent validation data suggested the possibility of using the LC-ESI/MS/MS method for simultaneous determination of low-level photoinitiator residues migrating from printed food-packaging materials into milk. The method has been successfully applied to the analysis of real samples of different fat contents ranging from 8 to 30 g L(-1). The photoinitiator residues were revealed to be higher in milk with higher fat content and the most important contaminations were benzophenone and ITX in concentration ranges of 2.84-18.35 and 0.83-8.87 microg kg(-1), respectively.

8.
J Sep Sci ; 32(23-24): 4020-4, 2009 Dec.
Artigo em Inglês | MEDLINE | ID: mdl-20066677

RESUMO

A method for the determination and confirmation of amitraz and its degradation product 2,4-dimethylaniline (2,4-DMA) in honey is reported. Determination of the two compounds was based on HPLC with UV detection and MS/MS (LC-MS/MS) after a liquid-liquid extraction with hexane and isopropyl alcohol. Chromatographic separation was achieved by using a C18 column with a gradient mobile phase consisting of 0.02 M ammonium acetate and ACN. Recoveries for fortified honey ranged from 83.4 to 103.4% for amitraz and from 89.2 to 104.7% for 2,4-DMA with RSD values lower than 11.6% for HPLC and LC-MS/MS methods. LOD was 6 microg/kg for amitraz and 8 microg/kg for 2,4-DMA, while LOQ was 20 microg/kg for amitraz and 25 microg/kg for 2,4-DMA in HPLC method. LOD was 1 microg/kg for amitraz and 2 microg/kg for 2,4-DMA, while LOQ was 5 microg/kg for amitraz and 10 microg/kg for 2,4-DMA in LC-MS/MS method.


Assuntos
Compostos de Anilina/análise , Cromatografia Líquida/métodos , Contaminação de Alimentos/análise , Mel/análise , Espectrometria de Massas em Tandem/métodos , Toluidinas/análise , Acaricidas/análise , Cromatografia Líquida de Alta Pressão/métodos , Resíduos de Praguicidas/análise , Espectrometria de Massas por Ionização por Electrospray/métodos
9.
J Sep Sci ; 32(23-24): 4193-9, 2009 Dec.
Artigo em Inglês | MEDLINE | ID: mdl-20066681

RESUMO

A method for the determination and confirmation of methylene blue (MB) in aquatic products was developed. Residues of MB were extracted from homogenized tissues with acetonitrile/sodium acetate buffer solution, and simply cleaned up with dichloromethane liquid/liquid extraction. After concentration and dissolution, the sample solutions were cleaned up by the neutral alumina and weak cation-exchange solid phase extraction (SPE) cartridge, prior to LC-MS/MS analysis. MB was determined at 1.0-20 microg/kg in eel, toasted eel and shrimp, with a limit of quantification of 0.5 microg/kg. Recovery for MB was between 73.0% and 108.3%. This method is fast, exact and sensitive. It can be applied to determine MB in aquatic products.


Assuntos
Cromatografia Líquida de Alta Pressão/métodos , Azul de Metileno/análise , Espectrometria de Massas em Tandem/métodos , Poluentes Químicos da Água/análise , Animais , Antifúngicos/análise , Aquicultura , Resíduos de Drogas/análise , Enguias , Concentração Máxima Permitida , Penaeidae , Extração em Fase Sólida
10.
Biomed Chromatogr ; 23(7): 740-4, 2009 Jul.
Artigo em Inglês | MEDLINE | ID: mdl-19319833

RESUMO

A highly sensitive method has been developed for the determination of urinary 7-aminonitrazepam (7-ANZP), the major metabolite of nitrazepam, using high-performance electrospray liquid chromatography tandem mass spectrometry. The samples were prepared for analysis by adding 7-aminoclonazepam (7-ACZP, internal standard), hydrolysis with beta-glucuronidase and liquid-liquid extraction. Mass spectral acquisition was achieved by selectively monitoring the reaction between the two diagnostic transition reactions. Qualitative analysis was based on the retention time, and the quantitation was carried out by comparison with the internal standard. The recoveries of different concentrations of 7-ANZP from spiked blank samples was 89.0-95.2%, and the relative standard deviation was below 6.4%. The limit of determination in urine was 0.07 ng/mL, and the limit of quantitation was 0.5 ng/mL in the linear range of 1-50 ng/mL. This method possesses the merits of convenient operation, high sensitivity and good repeatability, making it a practical method for analysis of 7-ANZP in urine.


Assuntos
Cromatografia Líquida de Alta Pressão/métodos , Nitrazepam/análogos & derivados , Espectrometria de Massas em Tandem/métodos , Clonazepam/análogos & derivados , Clonazepam/análise , Humanos , Modelos Lineares , Nitrazepam/metabolismo , Nitrazepam/urina , Reprodutibilidade dos Testes , Sensibilidade e Especificidade
11.
Se Pu ; 37(1): 8-14, 2019 Jan 08.
Artigo em Zh | MEDLINE | ID: mdl-30693703

RESUMO

A method is proposed for the simultaneous determination of nine benzimidazole and neonicotinoid pesticides present in honey by employing automatic solid-phase extraction with high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). A honey sample was dissolved in a phosphate buffer (pH=7.8) followed by ultrasonic extraction. The extracts were then purified through solid-phase extraction (SPE) with hydrophilic-lipophilic balance (HLB) cartridges. Finally, nitrogen was blown on the obtained mixture, and the mixture was subsequently filtered for conducting HPLC-MS/MS analysis. Nine compounds were detected under the multiple reaction monitoring (MRM) mode, and the corresponding quantification was performed by employing the method of internal standards. The nine detected pesticides demonstrated good linearity in the range of 0.002-0.05 mg/L, with the correlation coefficient values (r2) being higher than 0.99. The limits of detection (LODs) (S/N=3) and limits of quantification (LOQs) (S/N=10) were found to be in the ranges of 0.1-1.0 µg/kg and 0.3-2.0 µg/kg, respectively. Furthermore, the results indicated that the recoveries of the nine detected pesticides range from 78.2%-101.2% at three spiked levels of 5.0, 10.0, and 20.0 µg/kg with a relative standard deviation (RSD) range of 1.3%-14.3% (n=6). Hence, the proposed method is rapid and can be employed for accurate determination of pesticide residues in large quantities of honey samples.


Assuntos
Contaminação de Alimentos/análise , Mel/análise , Resíduos de Praguicidas/análise , Cromatografia Líquida de Alta Pressão , Extração em Fase Sólida , Espectrometria de Massas em Tandem
12.
Artigo em Inglês | MEDLINE | ID: mdl-18485838

RESUMO

A confirmatory method coupling liquid chromatography with tandem mass spectrometry (LC/MS/MS) was developed to determine the concentration of oxytetracycline (OTC), tetracycline (TC), chlortetracycline (CTC) and doxycycline (DC), which make up the tetracycline (TC) groups present in royal jelly. Sample preparation included deproteination, control of pH, extraction and clean-up on a solid-phase extraction (SPE) cartridge. The analyses were achieved by LC/MS/MS in selected reaction monitoring mode (SRM). The overall recovery of fortified royal jelly at the levels of 5.0, 10.0 and 40.0 microg/kg ranged from 62% to 115%, and the coefficients of variation ranged from 3.4% to 16.3% (n=6). The detection limits for TCs were under 1.0 microg/kg. The transformation between the TCs and its epimers (EpiTCs) was studied in standard solution and during the sample preparation process. This method can be used for the detection of tetracycline residues in royal jelly.


Assuntos
Antibacterianos/análise , Cromatografia Líquida/métodos , Resíduos de Drogas/análise , Ácidos Graxos/química , Espectrometria de Massas por Ionização por Electrospray/métodos , Espectrometria de Massas em Tandem/métodos , Tetraciclina/análise , Calibragem , Reprodutibilidade dos Testes , Sensibilidade e Especificidade
13.
Se Pu ; 35(10): 1068-1072, 2017 Oct 08.
Artigo em Zh | MEDLINE | ID: mdl-29048804

RESUMO

A method for the determination of characteristic compound 3,5-dimethoxybenzoate-4-diglucoside (leptosperin) in manuka honey was developed by automatic on-line solid phase extraction-liquid chromatography-high resolution mass spectrometry (SPE-LC-HRMS). The samples were separated on a Dikma Diamonsil Plus C18 column (150 mm×4.6 mm, 5 µm) using the mobile phases of 0.1% (v/v) formic acid aqueous solution and acetonitrile with gradient elution. The compound was detected with negative electrospray ionization (ESI-) in Target-MS2 mode. The results showed that the linear range was 0.5-100.0 mg/L, the correlation coefficient was 0.9993. The limit of detection (LOD, S/N ≥ 3) and limit of quantification (LOQ, S/N ≥ 10) of the method was 3 mg/kg and 10 mg/kg, respectively. The recoveries at the spiked levels of 50.0, 100.0, 200.0 mg/kg (10.0, 20.0, 50.0 mg/kg in black locust samples) were in the range of 82.0%-95.2% with the relative standard deviations ranging from 2.7% to 9.7% (n=6). The proposed method was applied to 95 mature honey samples from hives in New Zealand including 12 different kinds and 50 commercial honey samples from four different countries. The method is fast, sensitive and accurate to provide technical support to solve the judgment of the manuka honey imported from New Zealand.


Assuntos
Cromatografia Líquida de Alta Pressão , Ácido Gálico/análogos & derivados , Glicosídeos/análise , Mel/análise , Extração em Fase Sólida , Cromatografia Líquida , Ácido Gálico/análise , Nova Zelândia , Espectrometria de Massas em Tandem
14.
J AOAC Int ; 89(5): 1432-6, 2006.
Artigo em Inglês | MEDLINE | ID: mdl-17042196

RESUMO

A liquid chromatographic/tandem mass spectrometric method was developed and validated for the determination of chloramphenicol (CAP) in royal jelly. Royal jelly samples were first denatured with lead acetate solution, and the CAP was extracted with solid-phase extraction before separation by liquid chromatography. A triple-quadrupole mass spectrometer operated in the negative electrospray ionization and selected-reaction monitoring mode was used for the detection of CAP. For method validation, royal jelly samples were fortified at CAP levels between 0.1 and 10.0 microg/kg; at these levels, recovery values (internal standard-corrected) ranged from 93.3 to 105.0%, and the within-laboratory reproducibility (relative standard deviation) was < or = 9.1%. The decision limit was 0.07 microg/kg, and the detection capability was 0.1 microg/kg.


Assuntos
Antibacterianos/análise , Cloranfenicol/análise , Cromatografia Líquida/métodos , Ácidos Graxos/análise , Análise de Alimentos/métodos , Contaminação de Alimentos/análise , Espectrometria de Massas por Ionização por Electrospray/métodos , Antibacterianos/normas , Cloranfenicol/normas , Cromatografia Líquida/normas , Cromatografia Líquida/estatística & dados numéricos , Ácidos Graxos/normas , Análise de Alimentos/normas , Análise de Alimentos/estatística & dados numéricos , Contaminação de Alimentos/estatística & dados numéricos , Padrões de Referência , Reprodutibilidade dos Testes , Espectrometria de Massas por Ionização por Electrospray/normas , Espectrometria de Massas por Ionização por Electrospray/estatística & dados numéricos
15.
Se Pu ; 33(10): 1040-5, 2015 Oct.
Artigo em Zh | MEDLINE | ID: mdl-26930960

RESUMO

A method of high performance liquid chromatography-quadrupole/electrostatic field Orbitrap high resolution mass spectrometry (HPLC-Q/Orbitrap MS) was developed to determine fructo-oligosaccharides in milk powder. The milk powder samples were dissolved in deionized water. Subsequently, an aqueous solution of zinc acetate was used to precipitate protein. After centrifugation, the final aqueous solution was filtered by a polytetrafluoroethylene (PTFE) membrane with pore size of 0.22 µm. The analytes were separated on a Carbohydrate column (100 mm x 2.1 mm, 2.6 µm) through gradient elution with the combination of acetonitrile and 0.1% formic acid aqueous solution. The target-MS/MS templates were performed at isolation window of m/z 4.0 and collision energy of 30 eV in positive mode to extract the accurate product ion mass of analytes. Under the optimal condition, 1-kestose (GF2), nystose (GF3) and 1-F-ß-fructofuranosyl nystose (GF4) were well separated and the accuracy of extracted mass routinely detected was below 5 x 10(-6) (5 ppm). The whole analysis time is only ten minutes. The detection limits for GF2 and GF3 were 100 µg/kg, and the detection limit for GF4 was 55 µg/kg. Good linearities were obtained in their respective linear ranges with correlation coefficients higher than 0.998. The average recoveries at three spiked levels (5, 10 and 20 mg/kg) were in the range of 75.8%-107.3% and the relative standard deviations (RSDs) were in the range of 1.6% - 8.3%. The proposed method is simple, sensitive, fast and only in need of precipitation of proteins. The interference of matrix can be eliminated through the selection of product ion. The results were convenient and reliable and thus can be used in the large batch determination of any milk powder.


Assuntos
Leite/química , Oligossacarídeos/análise , Animais , Cromatografia Líquida de Alta Pressão , Espectrometria de Massas em Tandem
16.
Se Pu ; 33(7): 711-4, 2015 Jul.
Artigo em Zh | MEDLINE | ID: mdl-26672199

RESUMO

A method for the determination of three coriaria lactone residues in honey was developed using ultra high performance liquid chromatography-high resolution mass spectrometry. The honey samples were extracted with 0.2 mol/L phosphate buffer solution (pH = 7.5), and the extracts were cleaned up with Waters HLB solid phase extraction cartridges. The extracted components were separated on a Phenomenex C18 column by gradient elution. The qualitative and quantitative analyses were operated under t-MS2 by high resolution mass spectrometry. The results showed that the limits of detection and quantification for the three coriaria lactones in a spiked blank honey were 0.05 mg/kg and 0.1 mg/kg, respectively. The recoveries of the three coriaria lactones spiked in blank honey samples at the levels of 0.1 to 0.5 mg/kg were 86.3%-95.6% with the RSDs of 3.0%-8.4%. The method was applied for the determination of the manuka honey from New Zealand, and tutin was detected in one of the samples. The results showed that the method is suitable for the determination of the three coriaria lactone residues in honey.


Assuntos
Mel/análise , Lactonas/análise , Cromatografia Líquida de Alta Pressão , Espectrometria de Massas
17.
Se Pu ; 32(2): 189-93, 2014 Feb.
Artigo em Zh | MEDLINE | ID: mdl-24822456

RESUMO

An HPLC method was developed for the determination of methylglyoxal in Manuka honey of New Zealand. The honey sample was dissolved in water and mixed with o-phenylenediamine solution for derivatization. After the reaction for at least 8 h in the dark at room temperature, the solution was filtered with 0.22 microm membrane and injected into an HPLC system for analysis. The separation was carried out on a Kromasil reversed phase column with gradient elution. The mobile phases were methanol and 0. 1% (v/v) acetic acid aqueous solution. The detection wavelength was 318 nm. The external standard method was used for quantitation. The linear range of methylglyoxal was 1-50 mg/L with a correlation coefficient of 0. 999 9. The LOD (S/N = 3) and LOQ (S/N = 10) were 0.02 mg/L and 0.06 mg/L, respectively. The recoveries at the spiked levels of 50, 100, 200 mg/kg were 98.3%-101.5% and the RSDs (n = 5) were less than 5%. The derivative of methylglyoxal was stable within 24 h. The results showed that the pretreatment of this method is simple and the sensitivity, the recovery and repeatability are good. This method can be used for the quality control of Manuka honey of New Zealand, and also for the detection of methylglyoxal in Chinese honey.


Assuntos
Mel/análise , Aldeído Pirúvico/análise , Cromatografia Líquida de Alta Pressão , Nova Zelândia
18.
Se Pu ; 32(3): 314-7, 2014 Mar.
Artigo em Zh | MEDLINE | ID: mdl-24984475

RESUMO

A confirmatory method was established for the determination of trifluralin residue in aquatic products and edible oils with the technique of offline disperse solid phase extraction and gas chromatography-negative chemical ionization mass spectrometry (DSPE-GC-MS/NCI). Trifluralin was extracted from aquatic products and edible oils with acetonitrile, and liquid-liquid partitioning formed by adding anhydrous magnesium sulfate followed by a simple cleanup step known as dispersive solid-phase extraction. The aliquot was analyzed by GC-MS/NCI using isotope internal standard method. The method was reliable and stable. The recoveries of trifluralin were in the range from 80% to 100% at three spiked levels of 1.0, 2.0, and 3.0 microg/kg, and the RSDs were not more than 10.3%. The linearity of method was good from 1 to 40 microg/L, and the LOD was 0.02 microg/kg. This method can be used as a conclusive evidence method for the determination of trifluralin residue in aquatic products and edible oils.


Assuntos
Contaminação de Alimentos/análise , Resíduos de Praguicidas/análise , Trifluralina/análise , Cromatografia Gasosa-Espectrometria de Massas , Óleos/análise , Alimentos Marinhos/análise , Extração em Fase Sólida
19.
Se Pu ; 32(7): 741-5, 2014 Jul.
Artigo em Zh | MEDLINE | ID: mdl-25255567

RESUMO

A method was developed for the determination of four insecticide residues in honey and royal jelly by gas chromatography-negative chemical ionization mass spectrometry (GC-NCI/MS). The honey and royal jelly samples were treated with different preparation methods as the result of the different components. The honey sample was extracted with ethyl acetate and cleaned up with primary second amine, and the royal jelly sample was extracted with acetonitrile-water (1:1, v/v), and cleaned up with a C18 solid-phase extraction column. Finally, the extracts of the honey and royal jelly were analyzed by GC-NCI/MS in selected ion monitoring (SIM) mode separately. External standard calibration method was used for quantification. The linearities of calibration curves of the four insecticides were good with the correlation coefficients greater than 0.99 in the range of 50-500 microg/L. The limits of the detection (LODs) of the four insecticides were in the range of 0.12- 5.0 microg/kg, and the limits of the quantification (LOQs) were in the range of 0.40-16.5 microg/kg. The recoveries of the four insecticides spiked in honey and royal jelly at three spiked levels (10, 15 and 20 microg/kg) were in the range of 78.2 -110.0%, and the relative standard deviations (RSDs) were all below 14%. The sensitivity and selectivity of this method were good with no interfering peaks. The proposed method is simple quick and effective to analyze the four insecticide residues in honey and royal jelly.


Assuntos
Ácidos Graxos/análise , Mel/análise , Inseticidas/análise , Resíduos de Praguicidas/análise , Cromatografia Gasosa , Cromatografia Gasosa-Espectrometria de Massas , Limite de Detecção , Extração em Fase Sólida
20.
Se Pu ; 31(11): 1046-50, 2013 Nov.
Artigo em Zh | MEDLINE | ID: mdl-24558838

RESUMO

A liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed for the determination of five pyrrolizidine alkaloids (PAs) (monocrotaline, senkirkine, retrorsine, seneciphylline and senecionine) in honey. The honey samples were dissolved in 0.1 mol/L hydrochloric acid solution and a strong-cation exchange column was used to purify and concentrate the target analytes. The separation of the analytes was carried out on a Phenomenex C18 column (100 mm x 4.6 mm, 2.6 microm) using the mobile phases of acetonitrile and 5 mmol/L ammonium acetate-0.1% (volume percentage) formic acid aqueous solution with gradient elution. The separated compounds were detected in multiple reaction monitoring (MRM) mode via positive electrospray ionization (ESI+). The calibration curves were of good linearity in the range of 1-100 microg/L (r > 0.99). The limit of quantification of the method was 1.0 microg/kg. The average recoveries were between 73.1% to 107.1% at three spiked levels (1, 20 and 50 microg/kg) with the relative standard deviations (RSDs) in the range of 4.1% to 17.0%. The proposed method was applied to different kinds of honey from China, New Zealand, Spain and Australia. The samples included rape, vitex, sunflower, cotton, tilia tree, date, acacia, buckwheat, manuka and eucalyptus honey. Monocrotaline, senkirkine and retrorsine were not detected in the collected honey samples. However, seneciphylline and senecionine were found in most of the honey samples. The concentrations of seneciphylline and senecionine were 11.0 -31.1 microg/kg and 8.3-29.1 microg/kg, respectively.


Assuntos
Cromatografia Líquida , Mel/análise , Alcaloides de Pirrolizidina/análise , Espectrometria de Massas em Tandem
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