最新刊期
卷 35 ， 期 2 ， 2016
- 摘要：A comprehensive analytical method was developed and validated for the simultaneous determination of 53 kinds of glucocorticoids in facial mask cosmetics using solid-phase extraction(SPE) coupled with liquid chromatography-tandem mass spectrometry(LC-MS/MS).Cosmetic sample was dispersed with water，and the analytes were extracted with methanol by vortex mixer.The extracts were cleaned up with a Cleanert PEP(60mg,3mL) solid phase extraction cartridge after diluted with water. Electrospray ionization mass spectrometry was performed in the positive mode using dynamic multiple reaction monitor(DMRM) mode for the qualitative and quantitative analyses of 53 kinds of analytes after separation on a column of Waters CORTECS C18+(100mm×2.1mm，2.7μm).The correlation coefficients for linear calibration curves were over 0.99 in the corresponding concentration range.The average recoveries of 53 drugs from spiked sample at three different concentration levels ranged from 66.8%to 106.3%, with relative standard deviation(RSDs)of 3.9%-13.2%.The limits of detection(LODs,S/N≥3) and quantitation(LOQs,S/N≥10) were 3μg/kg and 10μg/kg, respectively.The established method is simple,reliable,accurate and sensitive,and is suitable for the determination of glucocorticoids illegally added in cosmetics.关键词：cosmetics;glucocorticoids;solid-phase extraction(SPE);liquid chromatography-tandem mass spectrometry(LC-MS/MS);dynamic multiple reaction monitoring(DMRM);illegal addition
- 2313
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- 1424
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- 14
发布时间： - 摘要：Cosmetic has been one of the consuming goods which is closely related to people’s daily life.Thus,it is of great significance for the analysis and detection of the banned or restricted substances in cosmetic.Due to the complex matrix and serious interferences,it is difficult to realize the direct detection of target analytes in cosmetic.Therefore,sample pretreatment techniques are required for the separation and enrichment of the target analytes.In this paper,some sample pretreatment methods for cosmetic samples including liquid-liquid extraction,solid phase extraction, solid phase microextraction, liquid phase microextraction, microwave-assisted extraction and ultrasonic-assisted extraction,etc.are reviewed. Also, the future trends of pretreatment of cosmetic samples are prospected.关键词：cosmetic;sample pretreatment;review;research progress
- 2041
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- 1305
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- 13
发布时间： - 摘要：Gout is a highly heterogeneous disease which occurs only in human being,it would cause gouty arthritis,and even lead to disability.There could be obvious alterations of metabolites in the serum of the patient with gout,and the discovery of metabolic characteristics may be helpful for the clinical diagnosis and treatment of gout.A gas chromatography-mass spectrometry(GC-MS) based metabolic profiling method was employed to analyze the distinctive metabolic patterns of serum in gout patients.Serum samples collected from 29 gout patients and 26 healthy controls were analyzed.The principal component analysis(PCA) and partial least squares discriminant analysis(PLS-DA) were used to assess the metabolic data.Marked differences between gout patients and healthy controls were shown in PCA score plot.Variable importance for project values(VIP) and Student’s t-test were combined to pick out the significant metabolic changes.Compared with that of the control group,the serum metabolic characteristics of the gout group were featured by increased levels of metabolites related to nucleotide metabolism(hypoxanthine, uric acid and uridine),carbohydrate metabolism(2,3-dihydroxybutyrate, D-threitol, D-gluconic acid,myo-inositol,etc.) and amino acid metabolism(3-hydroxy- 3-methylbutyrate,L-ornithine and indole-3-lactic acid),decreased levels of lipids(monoethanolamine,glycerol,glyceric acid,etc.),glycine and hypotaurine.The preliminary results suggest that GC-MS based metabolic profiling method appears to be a useful tool in the exploration of the serum metabolic characteristics of gout.These revealed disease-associated metabolic perturbations involved in multiple metabolic pathways including purine metabolism and the urea cycle,which could help to elucidate the pathogenesis of gout and provide a potential aid for the accurate diagnosis or treatment of gout.关键词：gout;metabolomics;gas chromatography-mass spectrometry(GC-MS);serum
- 2026
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- 1240
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- 2
发布时间： - 摘要：The quality and safety of cosmetics have been drawing increasing public attention in recent years.Many cosmetic products of well-known brands have been detected to contain prohibited or restricted substances,which may cause harm to consumers rights and interests,and bring about significant economic losses to cosmetic enterprises.To avoid the occurrence of quality and safety accidents on cosmetics,researchers have been engaging in developing a series of analytical methods for the detection of hazardous chemical ingredients in cosmetics using a variety of testing techniques.In this paper,the advances in analytical techniques for the quality and safety of cosmetics in the past years were summarized,and some newly-developed techniques for the analysis of cosmetics were introduced,which may provide a theoretical support and a technical instruction for the researchers and inspectors in analysis of cosmetic products.关键词：cosmetics;quality and safety;prohibited and restricted substances;analytical techniques;review
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- 7
发布时间： - 摘要：1H NMR spectroscopy combined with multivariate statistical method was introduced in this paper to explore the regulation effect of Gandouling on basal ganglia injury in copper-laden rats.24 male Wistar rats were randomly divided into control group,model group and Gandouling group,with 8 rats in each group.The rat model was established by copper-laden method.From the 7th week of modeling,Gandouling group was given Gandouling formula via gavage.Compared with the control group,the index of apoptosis cells in basal ganglia of model group increased significantly(p<0.01),and glutamine,uridine and threonine in basal ganglia were increased(p<0.05) while mannitol,adenosine,N-acetylaspartate,glutamate, N-acetylglutamine asparagine, acetate, aspartate,myo-inositol and ATP were decreased(p<0.05).Compared with the model group,the index of apoptosis cells in basal ganglia of Gandouling group was significantly decreased(p<0.01),and glutamine,uridine,acetate and aspartate were reduced(p<0.05) while mannitol,adenosine,threonine,N-acetylaspartate,glutamate, N-acetylglutamine, asparagine,myo-inositol and ATP were elevated(p<0.05).The results showed that Gandouling could influence the metabolism of basal ganglia in copper-laden rats,which has a certain therapeutic effect on damage caused by copper.The mechanism may be restoration of the functions of neurons and glial cells,through adjusting the detoxification of ammonia and metabolism of excitatory amino acid neurotransmitter and interfering the energy metabolism.关键词：metabolic response;copper-laden;basal ganglia;Gandouling;1H NMR
- 2036
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- 1085
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- 1
发布时间： - 摘要：A method for the determination of four active constituents(i.e. 2,3,5,4′-tetrahydroxy stilbene-2-Ο-β-D-glucoside(THS-GLU), quercetin-3-rhamnoside(QR), rutin(RT)and naringin(NG))in hair growth cosmetics was developed by strong anion exchange-solid phase extraction(SPE) combined with ultra performance liquid chromatography quadrupole-time-of-flight mass spectrometry(UPLC-QTOF-MS).The sample was ultrasonically extracted with methanol,and purified with SPE(PAX,500mg/6mL) cartridge.Chromatographic separation was conducted on a UPLC CSH C18(2.1mm×50mm,1.7μm,Waters) column by gradient elution using methanol and 0.002% formic acid solution as mobile phases.The MS analysis was carried out in electrospray ionization operated in negative mode.THS-GLU,QR and RT were quantified by the external standard method.NG,which arised configuration conversion to naringin chalcone,was just identified by qualitative analysis.Under the optimal conditions, satisfactory linearities(r2>0.999) for three compounds were obtained for all analytes in the concentration range of 5-200μg/L.Limits of quantitation(S/N=10) were in the range of 0.03-0.1mg?kg-1.Recoveries at three spiked levels were in the range of 80.9%-104.7% with relative standard deviations(RSD,n=6) not more than 19.6%.This method was accurate and applicable,and was succcessfully applied in the determination of THS-GLU,QR,RT and the identification of NG in hair growth cosmetics.关键词：solid phase extraction(SPE);ultra performance liquid chromatography quadrupole-time-of-flight mass spectrometry(UPLC-QTOF-MS);hair growth cosmetics;active constituents
- 2036
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- 1193
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- 3
发布时间： - 摘要：Metabonomics (metabolomics)is a subject branch that focuses on the dynamic changes of molecular mass metabolites in complex samples of an organism.Its research concept is consistent with the holistic view and dynamic state view of Traditional Chinese Medicine (TCM).Therefore,metabonomics has been widely applied in research on TCM,and chromatography-mass spectrometry has become the main analytical technique of metabonomics.Therefore,the applications of chromatography-mass spectrometry in TCM metabonomics are reviewed, the advantages and disadvantages of different separation techniques are discussed,and the latest developments of TCM metabonomics in the past three years are emphasized.关键词：chromatography;mass spectrometry;traditional Chinese medicine;metabonomics;review
- 2374
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- 1205
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- 7
发布时间： - 摘要：A method was developed for screening of 12 kinds of glucocorticoids in cosmetics by high performance liquid chromatography-quadrupole/orbitrap high-resolution mass spectrometry（Orbitrap MS）.The samples were extracted with acetonitrile,and separated with an Acquity UPLC BEH C18（100mm×2.1mm，1.7μm） using a binary solvent system composed of 0.1% formic acid methanol solution and 0.1% formic acid water solution by gradient elution.Accurate mass number of target compound were got in full scan mode.Compared to accurate mass number in theory,the mass accuracy error was below 2×10-6.The screening list was built,and the database of secondory characteristic fragment ions for the glucocorticoids were added in screening option.Qualitative screen was achieved.The limits of detection（LOD） of the method ranged from 1μg/kg to 2μg/kg，and the limits of quantitation（LOQ） ranged from 3μg/kg to 5μg/kg．Satisfactory recoveries from 78.3% to 115.2% were obtained at spiked concentration levels of 10,20,40μg/kg,and the relative standard deviations（RSDs） were in the range of 1.0%-11.2%.The method could be used for the determination of glucocorticoid in cosmetics as a high-throughput and confirmatory method.关键词：ultra high performance liquid chromatography;orbitrap mass spectrometry（Orbitrap MS）;glucocorticoid;cosmetic
- 2140
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- 1201
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- 6
发布时间： - 摘要：Prohibited or restricted ingredients are often added into functional cosmetics.This kind of cosmetics not only cause damage to the interests and health of consumers，but also disrupt the market order.In this paper，analytical methods and pretreatment techniques for pharmaceutical substances(hormones，antibiotics)，preservatives，sunscreens and other hazardous substances in cosmetics，which could be found in the literature，are reviewed.The applications of the analytical methods，techniques and sample preparation are discussed，and the prospects for the development of cosmetic detection methods are outlooked.关键词：cosmetic;harmful substances;analytical method;review
- 1950
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- 1304
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- 6
发布时间： - 摘要：A liquid chromatography-tandem mass spectrometric（LC-MS/MS） method was developed for the determination of five organophosphate ester metabolites in river water samples.The filtered water samples were enriched and purified by solid phase extraction（SPE） using a HLB cartridges,and then eluted with 6 mL methanol.The eluent was concentrated to a volume of 0.5mL under gentle nitrogen stream and then diluted to 1mL by initial mobile phase（50% methanol）.Instrumental analysis was accomplished by HPLC-MS/MS under negative electrospray ion and multiple reaction monitoring（MRM） mode.Separation of the analytes was performed on a Luna Phenyl-Hexyl column,and a mixture of methanol and 50mmol?L-1 ammonium acetate solution was selected as mobile phase for gradient elution.The recoveries of five organophosphate ester metabolites in river samples were in the range of 57.8%-102% at a spiked concentration of 50ng?L-1 with relative standard deviations（RSD） of 2.8%-15.7%.At a spiked concentration of 10ng?L-1,the recoveries were in the range of 54.1%-83.6% with RSDs of 5.3%-19.5%.The instrumental detection limits（IDL） ranged from 0.002μg?L-1 to 1.15μg?L-1 and the method detection limits（MDL） ranged from 0.15ng?L-1 to 4.48ng?L-1.The matrix effect of river samples was also investigated in this study.The proposed method was successfully applied in the determination of organophosphate ester metabolites in lake water samples collected from Wuhan,Hubei.Except for DEHP,the other four OPEs metabolites were all detectable in lake water.The method showed good precision and accuracy,and was suitable for the analysis of five organophosphate ester metabolites in surface water samples.关键词：organophosphate ester metabolites;liquid chromatography-tandem mass spectrometry（LC-MS/MS）;river water;solid phase extraction
- 1968
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- 1323
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- 8
发布时间： - 摘要：To explore the differences in body metabolism of experimental animals，the serum samples of four batches of healthy SD rats raised in different periods were compared using proton nuclear magnetic resonance(1H NMR) based metabolomic approach combined with multivariate statistical analysis.The results showed that the contents of several serum metabolites in different groups，including citric acid，pyruvic acid，succinic acid，glutamine，dimethylglycine，changed slightly，while the amounts of alanine，arginine，isoleucine，lactic acid，3-hydroxybutyric acid and choline were fluctuant.Further metabolic pathways analysis showed that amino acid metabolism，ketone body metabolism and choline metabolism were fluctuant in different groups of SD rats.This study provided a new method for the evaluation on the consistency among the different groups of healthy SD rats，and laid a basis for further determination on the biomarkers in serum samples.关键词：metabolomics;serum;rats;biological samples;1H NMR
- 1966
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- 1626
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- 1
发布时间： - 摘要：A new method was established to determine 14 kinds of ultraviolet absorbers and antioxidants（including UV-0,UV-9,UV-71,UV-329,UV-326,UV-327,UV-234,UV-360,antioxidant 2246,425,TH-1790,3114,1010 and 1076） in plastic food packing materials by ultrasonic extraction combined with ultra high performance liquid chromatography（UPLC）.In the study,the plastic food packing materials were ultrasonically extracted with trichloromethane-methanol,and analyzed with C18 column，employing acetonitrile -0.1% formic water as mobile phases by gradient elution．All of the samples were detected with diode-array detector.The 14 analytes presented good linearities in the respective linear ranges,with correlation coefficients（r2） not less than 0.999 2.The quantitation limits（S/N=10） were in the range of 8.0 -33.0 mg/kg,the average recoveries（n=6） ranged from 83.6% to 116.2%,with relative standard deviations（RSD,n=6） of 1.3%-9.5%.The developed method,characteristic by simple pre-treatment procedure and satisfactory purification,was suitable for the simultaneous determination of 14 kinds of ultraviolet absorbers and antioxidants in plastic food packing materials.关键词：ultraviolet absorbers;antioxidants;plastic food packing materials;ultra high performance liquid chromatography（UPLC）
- 2166
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- 1369
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- 15
发布时间： - 摘要：A high performance liquid chromatography-tandem mass spectrometric(HPLC-MS/MS)method was developed for the determination of 16 perfluoroalkyl acids in textiles.Samples were extracted with methanol through ultrasonic method.The target ingredients were separated on a C18 column(100 mm×2.1 mm，2.7 μm) using a mixture of methanol-water system as mobile phase by gradient elution.The 16 perfluoroalkyl acids were analyzed by MS under multiple reaction monitoring mode(MRM).The linear ranges of 16 perfluoroalkyl acids were between 1 ng/mL and 1 000 ng/mL.The limits of quantitation were between 0.21 μg/m2 and 1.53 μg/m2.The recoveries ranged from 84.8%to 107.4%,with relative standard deviations(RSDs,n=6) not more than 7.2%.This method was fast,sensitive,accurate,precise and convenient to operate,and it was appropriate for the determination of perfluoroalkyl acids in textiles in routine tests.关键词：textile;perfluoroalkyl acids;high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS);determination
- 1843
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- 1561
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- 5
发布时间： - 摘要：An ultra high performance liquid chromatography-tandem mass spectrometric(UPLC-MS/MS) method was developed for the determination of 9 sedative hypnotic drugs(chormezanone,triazolam,alprazolam,estazolam,diazepam,nitrazepam,oxazepam,lorazepam,chlordiazepoxide) in health foods, and the dissociation pathways of nine drugs were studied by electrospray ion mass spectrometry.After extracted with methanol,the analyses were separated on a Zorbax SB-C18(3.5 μm,2.1 mm×150 mm) chromatographic column by gradient elution using a mixture of acetonitrile and 0.1% formic solution as mobile phase at a flow rate of 0.3 mL/min.Detection was performed by electrospray ionization in the positive ion mode under multiple reaction monitoring(MRM) mode,and quantified with matrix standard curve.As a result,the calibration curves for all target compounds were linear in the range of 0.5-50 μg/L with correlation coefficients(r2) larger than 0.99．The limits of quantitation(LOQ,S/N≥10) were in the range of 1.6-9.2 μg?kg-1.The recoveries for all the drugs were 78.1%-101.2%.The intra and inter day precisions values at three spiked levels were between 1.4%-9.7%and 2.0%-11.2%,respectively.With strong selectivity,high sensitivity,easy operation and rapid detection,this method could be used to detect 9 kinds of illegally added sedative drugs in health foods.Moreover,the study of mass spectrometric behaviours and ion fragmentation patterns of nine drugs could provide a reference for the qualitative identification and quantitative analysis.关键词：ultra high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS);functional foods;sedative hypnotic drugs;fragmentation
- 1974
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- 1171
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- 3
发布时间： - 摘要：Piperlonguminine,the effective composition of the Mongolian medicine Piper longum L.,has fluorescence and its fluorescence signal could be greatly enhanced by the surfactant Tween -20.The synchronous fluorescence spectroscopic method could eliminate the interference of the background fluorescence from serum samples on fluorescence spectra of piperlonguminine.According to this technique,a method was established for the determination of piperlonguminine in rat serum.The linear range of this method was in the range of 5.47×10-3-3.28 μg?mL-1,the detection limit for piperlonguminine was 1.20×10-3 μg?mL-1,and the relative standard deviation(RSD) was 2.7%.The method was successfully applied in the detection of piperlonguminine in rat serum amples,with recovery of 100.6%.关键词：piperlonguminine;micellar system;fluorescence spectrometry;serum
- 1957
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- 1183
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- 0
发布时间： - 摘要：A new method using three phase hollow fiber-liquid phase microextraction was developed for the determination of indole phytohormones in bean sprout by spectrofluorimetry.The parameters affecting liquid phase microextraction performance were optimized using L9(34)orthogonal experiment.The optimum extraction was achieved by adjusting sample solution pH value to 4.0, using 1-octanol as organic extraction solvent, pH 12.0 solution as acceptor phase, and stirring the solution at 1 000 r/min for 60 min.Under the optimum conditions, the calibration curve showed a good linearity(r=0.997 9) in the range of 1.71-50.0 mg/L, with a detection limit of 0.57 mg/L.Recoveries for spiked samples from 88.6%to 100.7%were obtained with RSDs not more than 4.8%.The proposed method was simple, green and accurate in the determination of indole phytohormones in bean sprout.关键词：hollow fiber three phase liquid phase microextraction;indole phytohormones;orthogonal experiment;spectrofluorimetry;bean sprout
- 2052
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- 1192
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- 2
发布时间： - 摘要：Rare earth elements(REEs) in geological samples are of great interest,mainly because they might be considered as a primary source with the potential to resolve the global REEs supply shortage.This paper describes a method for the determination of REEs in geological samples by inductively coupled plasma mass spectrometry(ICP-MS).Samples were dissolved using distilled HNO3 and HF during microwave digestion process,in which HNO3 was added after acid-drying.The whole process was safe and efficient without any loss.In addition,the use of ICP-MS could effectively eliminate the interference of polyatomic ions.After optimizing the instrument parameters,the internal standard element rhodium(Rh) was used to compensate for matrix suppression effect and sensitivity drift so that the results were more accurate.The method was applied in the determination of REEs in the National Geochemistry Standard Reference Materials(GBW07109,GBW07110 and GBW07111).The determined values are in good agreement with the certified values.The results show that this method has the advantages of simplicity,rapidness, low detection limit and high accuracy，and could be used for the detection of many different elements at the same time．关键词：microwave digestion;inductively coupled plasma mass spectrometry(ICP-MS);geological samples;rare earth elements
- 2055
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- 3
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- 24
发布时间： - 摘要：A biosensor for dimethoate was prepared by exploiting their inhibitory effect on the activity of acetylcholinesterase(AChE).Carbon/Pt sphere material with good chemical stability, large surface area and good conductivity was used to modify the electrode.Compared to a bare electrode, the electron transfer resistance of the prepared electrode is lower,and its peak current is increased by 147.06%.This is ascribed to the larger surface of the Carbon/Pt ball material which could improve theadsorption for AChE and enhance its activity.Under the optimal experimental conditions , the concentration of negative logarithm of dimethoate and inhibition ratio showed a good linear relationship from 1.0×10-9 g/L to 1.0×10-6 g/L.The detection limit was 7.3×10-12g/L(the inhibition rate was 10%).The spiked recoveries for textile samples were in the range of 86.2%-101.7%.The method may provide a new way to fabricate highly sensitive biosensors for the detection of organophophate pesticides in textile.关键词：Pt/Porous carbon spheres;biosensor;acetylcholinesterase;dimethoate;textile
- 2021
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- 1150
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- 3
发布时间： - 摘要：A solid phase microextraction(SPME) coupled with gas chromatography-mass spectrometry was developed for the determination of N-nitroso-N-methylaniline(NMPhA)，N-nitroso-N-ethylamine(NEPhA) and N-nitrosodiphenylamine(NDPheA) in rubber sealing material.The samples were pretreated by GB/T 24153-2009 standard method，and then extracted by SPME.Influences of fibers species，extraction time，mixing speed and temperature on extraction efficiencies of three N-nitrosamines were optimized.Under the optimized experimental conditions，the linear ranges of NMPhA，NEPhA and NDPheA were between 5 μg/L and 500 μg/L with correlation coefficients(r) larger than 0.99. The method detection limits were 0.5 μg/kg.The average recoveries were in the range of 77%-92% with relative standard deviations(RSD，n=6) of 3.8%-7.7%.关键词：rubber sealing material;solid-phase microextraction;gas chromatography-mass spectrometry;N-nitrosamine
- 2118
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- 1383
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- 9
发布时间： - 摘要：Due to the edges containing a large number of functional groups(such as carboxyl groups),graphene oxide sheet could be effectively used to form a nuclear site and used as a template for biomimetic synthesis.In this paper,the application of graphene oxide used as the template for biomimetic synthesis of organic/inorganic hybrid materials was reviewed.The fundamental principle was introduced，and the preparation methods of different types of hybrid materials were summarized.The new trends of graphene based organic/inorganic hybrid materials were discussed.关键词：graphene oxide;biomimetic synthesis;hybrid materials;review
- 1995
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- 1335
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- 3
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