摘要:A QuEChERS/high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) was established for the determination of 90 nafils illegally added into distilled liquor and its products.The distilled liquor and its products samples were extracted with methanol solution,followed by purification of matrix dispersion solid phase extraction.The supernatant was firstly passed through a 0.22 μm organic phase microporous filter membrane,then analyzed by liquid chromatography-tandem mass spectrometry with electrospray ionization(ESI) ion source in positive ion mode under multi-reaction monitoring(MRM) mode.The retention time and ion ratio were used for qualitative analysis and the external standard method was adopted for quantification.The accuracy and precision of the method were verified by taking white spirit,Brandy and ginseng wine as sample matrices.The results showed that 90 kinds of illicit drugs could be satisfactorily separated within 20 min under the above chromatographic and mass spectrometric conditions,and the linearities were good in the range of 0.05-50 μg/L,with correlation coefficients(r2) greater than 0.999.The limits of detection(LODs) of the method were in the range of 0.5-10.0 μg/kg,and the limits of quantitation(LOQs) were 1.25-25.0 μg/kg.The recoveries for the analytes at different spiked levels ranged from 78.3% to 109%,with relative standards deviations(RSDs) of 1.2%-9.9%.The method was applied to the determination of 90 nafils in 47 batches of distilled liquor and its products.The results showed that sildenafil is contained in 2 batches of samples.With the advantages of simplicity in pretreatment,good purification effect on complex liquor matrix,and stable recovery,this method could be used for the rapid and simultaneous detection of 90 nafils illegally added substances in distilled liquor and its products.
关键词:high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS);QuEChERS;distilled liquor and its products;nafils;illegal addition
摘要:A method was established for the high-throughput and rapid analysis of characteristics chemical components in Brucea javanica oil and its oral drugs by direct injection electrospray ionization ultra high resolution mass spectrometry(DI-ESI-UHRMS) combined with statistical data analysis strategy.Based on the characteristics of DI-ESI-UHRMS with high resolution,high-throughput and non-targeted,69 accurate molecular formulas were resolved(the error with theoretical value is less than 1 ppm) in positive ion mode by analysis of the accurate mass number and fine isotope peak information for Brucea javanica oil and soybean lecithin soft capsule.Combining data from secondary mass spectrometry,literature,and Lipid Maps website,semi-identification of 69 accurate molecular formulas was performed,which were carbohydrates,phospholipids,oleic acids and oils composition.The results of component analysis(PCA),orthogonal partial-least squares discriminant analysis(OPLS-DA) and hierarchical cluster analysis(HCA) showed that Brucea javanica oil,olive oil and canola oil did not contain phospholipids,and the mother peak(m/z) corresponding to 69 semi-identified molecular formulas could be used as the index component for the identification of false adulteration of Brucea javanica oil and the difference analysis of oral preparations.This study provides a theoretical support for further improving the quality standards of Brucea javanica and its preparations.
关键词:Brucea javanica oil;oral drugs;characteristics;direct injection electrospray ionization ultra high resolution mass spectrometry(DI-ESI-UHRMS);high-throughput
摘要:A dehydroabietic acid glycidyl methacrylate ester(DAGME)-bonded silica stationary phase(Sil-DAGME) was fabricated in this paper.The DAGME was firstly prepared using dehydroabietic acid and glycidyl methacrylate via a ring-opening addition reaction,and then grafted onto the surface of a thiol-functionalized spherical silica by click reaction to obtain the Sil-DAGME.The successful immobilization of DAGME on the silica was confirmed through series of characterizations including Fourier-transform infrared spectroscopy(FT-IR),thermal gravimetric analysis(TGA) and elemental analysis(EA).The chromatographic performance and retention mechanisms of Sil-DAGME were validated using a variety of compounds including alkylbenzenes,Tanaka standard test mixtures,polycyclic aromatic hydrocarbons,phenols and flavonoids.Meanwhile,the Sil-DAGME exhibits multiple interactions,including hydrophobic,π-π and hydrogen bonding interaction between the stationary phase and the analytes during the separation process due to the co-existing of benzene ring,carbonyl group,hydroxyl group and hydrophobic rigid tricyclic hydrophenanthrene skeleton in the DAGME on the silica surface.Based on synergistic action of multiple retention mechanisms,the probe molecules metioned above achieved ideal resolution and flexible selectivity in separation.In addition,the Sil-DAGME not only exhibited good stability,repeatability and reproducibility with the run-to-run relative standard deviations(RSDs) of 0.050%-0.19%(n = 10),the day-to-day RSDs of 0.25%-1.0%(n = 7),and the column-to-column RSDs of 0.78%-2.1%(n = 3) for the retention time,but also showed an excellent separation ability for Yew tree bark extract.In short,the application of dehydroabietic acid in chromatographic separation materials not only provided a new approach for the separation and detection of paclitaxel,but also presented a reference for the design stationary phase using natural product rosin as functional ligand.
摘要:A ratiometric fluorescent sensor for genetically modified components was constructed using fluorescence resonance energy transfer(FRET) nanotags combined with catalytic hairpin assembly(CHA) enzyme-free amplification signal amplification pathway in this paper.First,two sequences HP1 and HP2 with hairpin structures were designed for CaMV35S(tDNA)-induced CHA,and then based on the FRET effect,AgNCs and CDs came in close proximity when single-stranded DNA labeled carbon dots(sDNA-CDs) and DNA templated silver nanoclusters(Ts-AgNCs) were hybridized,which led to the fluorescence quenching of CDs.A ratiometric fluorescent probe with sDNA-CDs/Ts-AgNCs fluorescence quenching is obtained.When tDNA is present,through the base complementary pairwise hybridization reaction,tDNA opens the HP1 hairpin to form an HP1-tDNA double-stranded structure.This structure can open the HP2 hairpin structure,thus forming an HP1-HP2 double-stranded structure,in which the tDNA was released into the next round of hybridization,triggering the CHA cycle.Since the affinity between the partial sequence of HP1 and the partial sequence of Ts in HP1-HP2 was stronger than that of sDNA,the fluorescence of CDs(λem = 464 nm) was enhanced by the release of sDNA-CDs from the probe after the addition of sDNA-CDs/Ts-AgNCs.However,AgNCs were still remained in the double-chain structure,leading to the unchanged fluorescence intensity of AgNCs(λem = 560 nm).Under the optimal conditions,the output signal of IF464/IF560 showed a linear relation for CaMV35S in the concentration range of 0.1-50 nmol/L,and the detection limit(LOD,S/N = 3) was calculated to be 0.02 nmol/L.The prepared probe was used for the detection of CaMV35S components in transgenic tomato leaves with good selectivity and reliable results.
摘要:An analytical method for the determination of tacrolimus(TAC) in blood plasma was established by supramolecular solvent(SUPRAS) extraction combined with ultra-high performance liquid chromatography-tandem mass spectrometry.After optimizing the key factors such as the composition and amount of SUPRAS,and vortex extraction time through single factor experiment and response surface design,blood plasma samples were extracted efficiently with SUPRAS formed by pentanol,tetrahydrofuran and water.The extract was separated on a Waters ACQUITY UPLC BEH C18 column(50 mm × 2.1 mm,1.7 μm),analyzed by electrospray ionization mass spectrometry in positive ion mode under multiple reaction monitoring(MRM) mode,and quantified by internal standard method.Experimental results demonstrated that there was a good linear relationship for TAC in the concentration range of 0.5-30 ng/mL,with a correlation coefficient(r) of 0.998 6.The limit of detection(LOD) and quantitation(LOQ) were 0.1 ng/mL and 0.5 ng/mL,respectively.The average recoveries(n = 3) at low,medium and high spiked concentration levels ranged from 91.9% to 99.9%,with relative standard deviations(RSDs) of 1.7%-5.7%.The proposed method is rapid,sensitive and stable,and it was suitable for the accurate determination of TAC in blood plasma.
关键词:tacrolimus;immunosuppresive agent;supramolecular solvent;plasma;ultra-high performance liquid chromatography-tandem mass spectrometry
摘要:Liquid chromatography-high resolution mass spectrometry was ultilized for the analysis on 21 metabolites of ADB-BUTINACA in zebrafish over different time periods in this paper.Firstly,the partial least squares discriminant analysis and hierarchical clustering analysis of orthogonal signal transformation were used to screen out 7 metabolites with significant differences between groups.Furthermore,a Stacking integrated learning model was established with the 7 differential metabolites as the characteristics for classification and prediction on 4 groups of samples in zebrafish in different time periods.It was found that the prediction accuracy of the model was as high as 98%,indicating that the potential differential metabolites screened could effectively reflect the variation of the original drug in zebrafish in different time periods.The content changes of metabolites in the 4 groups of samples were enriched and analyzed.The results showed that the overall content of differential metabolites decreased with the increase of exposure time,and the content distribution of various metabolites tended to be balanced from the initial imbalance.In addition,the experiment showed that most of the differential metabolite metabolic pathways closely related to hydroxylation reactions,and it was speculated that the hydroxylation reactions of the original drug in vivo had a certain correlation with the estimation of administration time. The experimental results could provide a basis for analysis in related fields such as drug taking time estimation.
关键词:ADB-BUTINACA;differential metabolites;Stacking integrated learning;metabolic pathway;enrichment analysis;liquid chromatography-high resolution mass spectrometry
摘要:A kind of novel ethylenediamine hybrid zinc germanate nanoribbons(NH2-Zn2GeO4 NRs) for adsorption and detection of uranyl ions was synthesized by hydrothermal synthesis.The structure and optical properties of NH2-Zn2GeO4 NRs were characterized by transmission electron microscopy(TEM),Fourier transform infrared spectroscopy(FTIR),X-ray photoelectron spectroscopy(XPS),X-ray diffraction(XRD),thermogravimetric analysis(TG),X-ray energy spectrometry(EDS),ultraviolet-visible absorption spectrum(UV-Vis) and fluorescence spectroscopy.The results showed that the NH2-Zn2GeO4 NRs have a crisscross band structure with good crystallinity and good thermal stability.Meanwhile,the surface of NH2-Zn2GeO4 NRs contains rich amino groups,greatly improving the dispersion of the nanoribbons and facilitating the coordination of UO with the surface amino groups,and then adsorbing UO.Furthermore,the interaction between the —Ge—O—H group on the surface of zinc germanate nanoribbons and UO,based on the antenna effect,turns on green fluorescence to realize the fluorescence detection of UO.Therefore,the NH2-Zn2GeO4 NRs could selectively and efficiently adsorb UO,and their adsorption of uranyl ions conforms to Langmuir isotherm model,with a maximum adsorption capacity of 190 mg/g.On the other hand,a sensitive detection method for UO was established based on the interaction between UO and NH2-Zn2GeO4 NRs,which could turn on green fluorescence,with a linear range of 0-45 μmol/L and a detection limit as low as 0.202 μmol/L.Results showed that only UO can make NH2-Zn2GeO4 NRs solution produce green fluorescence,while other ions have no fluorescence enhancement effect,indicating that the nano material has high selectivity and strong anti-interference ability.The method was successfully applied to the concentration analysis of UO in tap water,lake water,river water and sea water.The recoveries for the actual samples ranged from 87.2% to 102%,with the relative standard deviations less than 10%.Therefore,the prepared NH2-Zn2GeO4 NRs could be used for the simultaneous adsorption and detection of UO,which has a wide application value in detection of actual water samples.
摘要:A rapid analytical method for detection of chemical components in white tea and Pu’er raw tea was established based on ultra-high performance liquid chromatography-quadrupole-Orbitrap high-resolution mass spectrometry(UHPLC-Q-Orbitrap-HRMS) in this paper.The tea extracts were separated on a Waters ACQUITY UPLC BEH C18 column(150 mm × 2.1 mm,1.7 μm),and then analyzed by Q-Orbitrap-HRMS.Full scan/dd-MS2 was used in both positive and negative ionization modes for data acquisition.Based on the accurate mass information of precursor and fragment ions and online database matching,a total of 64 active ingredients and 32 common active ingredients were identified in the white tea and Pu’er raw tea samples,in which 16 active ingredients were identified only in white tea samples,while another 16 active ingredients solely occurred in Pu’er raw tea samples.They were mainly classified into six categories,including amino acids,organic acids,flavonoids,coumarins,alkaloids and nucleosides.The normalization method was used to determine the relative contents of the 64 active ingredients.This method could be used to analyze the active components in tea,providing a scientific basis for further research on the health mechanism of white tea and Pu’er raw tea,and also providing a technical support for the supervision of tea quality and safety.
关键词:ultra-high performance liquid chromatography;high-resolution mass spectrometry;white tea;Pu’er raw tea
摘要:An ultra-high performance liquid chromatography-quadrupole time-of-flight mass spectrometry(UPLC-Q/TOF MS) was applied to establish a metabolic map on the serum samples of 60 healthy volunteers(control group) and 65 gout patients(gout group),to investigate the serum metabolomics differences between patients suffering from gout and healthy volunteers to find potential serum biomarkers.The obtained data were pattern-identified based on principal component analysis and orthogonal partial least squares analysis.The serum metabolic markers for gout patients were screened by the combination of variable weight projection analysis and a volcanic map.Through data analysis and database search,a total of 63 different metabolites were screened,27 metabolites were significantly up-regulated(P < 0.05),while 36 metabolites were significantly down-regulated(P < 0.05),mainly including glycerol phospholipids,amino acids and choline,etc.Firstly,conducting ROC curve analysis on the obtained differential metabolites,14 metabolites with AUC area greater than 0.8 were the better metabolites for diagnosis.Then,63 differential metabolites screened were analyzed for metabolic pathway enrichment.Impact > 0.1 and P < 0.05 were taken as the standards,the obtained metabolic pathway primarily included glycerol phospholipid metabolism,ether lipid metabolism,linoleic acid metabolism,cysteine and methionine metabolism,arachidonic acid metabolism and the mutual conversion of pentasaccharide and glucuronic acid.Results showed that there were apparent differences in serum metabolism levels between gout patients and healthy control populations,and the identification of differential metabolites provided an experimental basis for the pathogenesis and early screening of gout.
摘要:A general 1H nuclear magnetic resonance spectroscopic(1H qNMR) method was established for the quantification of 75 synthetic cannabinoid receptor agonists(SCRAs) in seized e-liquid samples in this paper.The key qNMR spectrum acquisition and processing parameters,such as spin-lattice relaxation time(T1),internal standard and SCRAs quantitative peak were thoroughly discussed.1,3,5-trimethoxybenzene was used as the internal standard,and the samples were directly analyzed after dilution with deuterated methanol.The limit of quantitation(LOQ) of this method was 0.03%,the intra-day relative standard deviation(RSD) was less than 0.90%,the inter-day RSD was less than 1.5%,and the spiked recoveries for the matrixes were in the range of 93.3%-100%.The developed method was applied to the quantification of four SCRAs,including N-(1-methoxy-3,3-dimethyl-1-oxobutan-2-yl)-1-(5-fluoropentyl)-1H-indazole-3-carboxamide(5F-ADB),methyl 2-(1-(5-fluoropentyl)-1H-indole-3-carboxamido)-3,3-dimethylbutanoate(5F-MDMB-PICA),methyl 2-(1-(4-fluorobutyl)-1H-indazole-3-carboxamido)-3,3-dimethylbutanoate(4F-MDMB-BUTINACA),and N-(1-amino-3,3-dimethyl-1-oxobutan-2-yl)-1-butyl-1H-indazole-3-carboxamide(ADB-BUTINACA) in 19 seized e-liquid samples.The contents of SCRAs ranged from 0.072% to 2.056%.To be specific,the content of 5F-ADB ranged from 0.081% to 0.200%(n = 3),the content of 5F-MDMB-PICA ranged from 0.072% to 1.453%(n = 7),the content of 4F-MDMB-BUTINACA ranged from 0.122% to 0.477%(n = 5),and the content of ADB-BUTINACA ranged from 0.561% to 2.056%(n = 4).The quantitative results for SCRAs in 19 e-liquids by 1H qNMR and high-performance liquid chromatography(HPLC) were compared using Wilcoxon signed-rank test.The test P value was 1.00,indicating that there was no significant difference between the quantitative results of these two methods.The proposed 1H qNMR method is simple and accurate,which does not require the SCRAs reference material.It solves the problem of quantitative analysis for SCRAs in complex matrix when there is no reference material.At present,there is no report on the quantitative analysis of 75 kinds of SCRAs in e-liquids by 1H qNMR.This study further broadens the application scope of 1H qNMR in the field of drug control,and provides a new idea for quantitative analysis of drugs and new psychoactive substances in complex matrix.
摘要:A portable fluorescence sensing platform based on pyronitrile(DCI) near-infrared probe 1a and WeChat applet was constructed for the detection of ONOO-.The near-infrared probe 1a was firstly designed and synthesized based on a DCI fluorescent derivative,which was used for specific detection of ONOO-.The probe itself possess orange fluorescence,and the probe’s phenylboronic acid pinacol ester structure sheds after stimulation with nitrite ONOO-,then the parent intramolecular charge transfer(ICT) effect is restored,resulting in enhanced fluorescence emission and a color change of the probe’s fluorescence from orange to red after activation. Meanwhile,probe 1a exhibited excellent selectivity and anti-interference ability,the ultra-low detection limit reached 97 nmol/L.In addition,a simple detection platform based on a WeChat mini program “Colorimetric acquisition” was established,relying on the correlation between luminous chrominance of probe and ONOO- fluorescence response to probe,which could be used to intelligently evaluate the detection effect of exogenous ONOO-.This detection platform has a potential to become a simple analysis tool for portable and intelligent detection of hazardous substances in the environment.In conclusion,the NIR dye-based probe 1a developed in this paper was applied to the detection of ONOO-,providing a new reference for the intelligent detection of hazardous substances.
摘要:Single-cell mass spectrometry analysis enables metabolic profiling of individual cells,helps to reveal the heterogeneity among cells,which is of great significance in oncology research.Bladder cancer is the most common malignant tumor in the urinary system at present.Accurate identification on the types of bladder cancer cells has an important value in life science and clinical application in the selection of treatment plan,prognosis judgment and drug resistance evaluation of patients.In this paper,single-cell mass spectrometry combined with machine learning was used to identify bladder cancer cells.The metabolic profiles for different bladder cancer cell subtypes were investigated by single-cell mass spectrometry analysis system,and classification algorithms were studied. Based on the collected single cell metabolic data,t-distributed stochastic neighbor embedding(t-SNE) clustering algorithm was used for dimensionality reduction analysis on the data,and the difference between the single cell metabolic profile was visualized in the two-dimensional space.In order to accurately identify different types of bladder cancer cells,linear discriminant analysis,random forest,support vector machine and logistic regression were respectively used to establish machine learning classification models,and grid search method and 5-fold cross-validation were used to optimize the model parameters.Then,five repeats of 10-fold cross-validation were performed on all data sets,and the averaged statistical result was taken as the final result.Accuracy,sensitivity,specificity,receiver operating characteristic(ROC) analysis and other indicators were used to comprehensively evaluate the performance of the model.The results showed that the metabolites of a single bladder cancer cell,such as ADP,ATP,glutamic acid,pyroglutamic acid,glutathione,etc,were successfully detected by the single-cell mass spectrometry system.There were significant differences among different types of bladder cancer cells,as well as large differences among single cells of the same type,indicating the high heterogeneity of single cell in the tumor.In addition,the four machine learning models all had good typing ability for bladder cancer cells,with a comprehensive accuracy not less than 94.9%,a sensitivity not less than 88.6% and a specificity not less than 93.3%.Compared with other methods,the random forest algorithm has the highest classification accuracy,sensitivity and specificity,which are all up to 100%,and the area under the ROC curve(AUC) of the model is up to 1,indicating that this method has obvious advantages in classification performance. The method presented in this paper realized the detection of metabolites and differentiation of cell subtypes at single cell level of bladder cancer,paving the way for more single cell metabolomics research in future.
关键词:single-cell mass spectrometry;bladder cancer;metabolite detection;cell typing
摘要:In this paper,a naked-eye magnetic molecularly imprinted photonic crystal sensor(MMIPCs) based on magnetic molecularly imprinted nanoparticles(MMINPs) for tetracycline(TC) detection was constructed,under the external magnetic field through magnetic assembly of the MMINPs.The MMINPs were prepared by one-step method through miniemulsion self-assembly,with oleic acid modified magnetite nanoparticles as the magnetic cores,the amphiphilic random copolymer P(St-co-VP) as both the emulsifier and coating,and TC as the template molecule.PVP molecular chain stretched outward to obtain a steric hindrance between magnetic colloidal nanoparticles(MCNPs) owing to the hydrogen bonding between the PVP and water molecules.A magnetic responsive photonic crystal based on steric hindrance rather than electrostatic interaction as the counterbalance to magnetic attraction was developed.During the self-assembly of the P(St-co-VP) aggregating on the surface of MCNPs,the target molecules were added,which were imprinted in the coatings of MCNPs,relying on the hydrogen bond between PVP and the templates without further polymerization reaction.The MMINPs was characterized by transmission electron microscopy(TEM),Fourier transform infrared spectoscopy(FT-IR) and thermal gravimetric analyzer(TGA).In FT-IR spectrum for MMINPs,the stretching vibration peaks of C—O indicated the successful imprinting of TC.TEM showed that the particles were regularly spherical and uniform in size distribution.The average particle diameter of the MMINPs was around 153.6 nm.TGA showed that the content of magnetic substance was high to 67.44%,which was ascribed to ferromagnetic substance (Fe3O4 or Fe2O3) with high thermal stability.The preparation conditions of TC-MMINPs were optimized and the sensitivity,response time and the selectivity of TC-MMIPCs sensors were also investigated.With the increase of concentration from 1.0 × 10-4 g/L to 1.0 g/L,the reflection wavelength of TC-MMIPCs redshifts from 500 nm to 578 nm.The logarithm of the concentration of TC exhibits a linear relationship with the reflection wavelength in this range.The detection limit(S/N = 3) was 1.0 × 10-4 g/L and the response equilibrium time of the TC-MMIPCs sensor did not exceed 30 s.Such a rapid response was attributed to the surface imprinting.The imprinting factor of the TC-MMIPCs was 3.41 and the response was specific with the selection factor of 5.92 for chloramphenicol,which is structurally similar to the tetracycline.TC-MMIPCs were successfully applied to determine TC in the actual samples.A brand of soothing moisturizing spray was analyzed,the TC content in the moisturizing spray was obtained based on the linear curve of the TC concentration and the reflection wavelength obtained previously,and no TC was detected in the moisturizing spray.
关键词:magnetic colloidal nanoparticles;magneto-responsive photonic crystal;molecular imprinting technology;tetracycline;amphiphilic random copolymer
摘要:A gas chromatography/combustion-isotope ratio mass spectrometry(GC/C-IRMS) with purge and trap technique(P&T) was developed for the determination of compound specific carbon isotopes of trace benzenes in water in this paper. Three experimental conditions(purge time,purge temperature and dry-blow time) of P&T were investigated,and the optimal P&T efficiency was determined.The detection limits for trace benzenes in water were calculated by testing aqueous solutions of benzene in different mass concentrations.The results showed that under the conditions of 13 min of purge trapping and 3 min of dry-blowing time at 35 ℃,the P&T efficiencies for each benzenes(benzene,toluene,ethylbenzene,m/p-xylene,o-xylene,styrene and isopropylbenzene) in water samples could reach 95.0%,90.2%,71.3%,59.1%,69.4%,50.8% and 70.1%,respectively,and the isotope standard deviations(STD) ranged from 0.06‰ to 0.29‰.There were good linear relationships for the peak areas of seven benzenes and their concentration in ranges of 0.50-20.00 µg/L,with their correlation coefficients(r2) of 0.998 6-0.999 5.The standard deviations for the monomeric carbon isotope values of the seven benzenes were in the range of 0.090‰-0.48‰ at each concentration,and the differences between injection concentration and methods could not lead to carbon isotope fractionation.The detection limits for benzene,toluene,m/p-xylene,o-xylene and styrene in water samples were 1.00 µg/L,while those for ethylbenzene and isopropylbenzene were 0.50 µg/L.The established method can greatly improve the detection limits for benzene monomer carbon isotopes in water with accurate and reliable results to meet the needs for analysis on the monomer carbon isotopes of trace benzene in water.
关键词:purge and trap technique;trace benzenes;compound specific carbon isotope analysis;water
摘要:A high performance liquid chromatographic(HPLC) method was established for the determination of 9 self-heating compounds,including capsaicin in cosmetics.The samples were ultrasonically extracted with 80% methanol,and then filtered.The target compounds were separated on a SymmetryShieldTMRP18(250 mm × 4.6 mm,5 μm) with a mobile phase consisting of acetonitrile and 0.5% formic acid by gradient elution,and analyzed by HPLC with a PDA detector.Under the optimal conditions,good linear relationships were obtained for nine compounds in the concentration range of 0.2-100 μg/mL,with correlation coefficients(r2) not less than 0.999 5.The limits of detection(LODs) were in the range of 0.001 0-0.003 4 mg/kg.The spiked recoveries for water,lotion and cream matrixes at three levels of 0.004,0.02,1 mg/kg ranged from 75.6% to 115%,with relative standard deviations(RSDs,n = 3) of 0.083%-7.0%.This method is accurate and sensitive,and is suitable for the qualitative and quantitative analysis of 9 self-heating compounds in cosmetics.
摘要:The widespread use of cosmetic products at home and abroad makes its safety problem attract extensive attention.As the first choice to find out the safety problem of cosmetic samples,analysis and detection technology is very important.Various morphology and complex matrix which cosmetic samples are characterized by bring great challenges to the detection of target analytes in cosmetics.Traditional sample pretreatment methods cannot meet the requirements for green and efficient detection due to the disadvantages of large reagent and time consumption,tedious preparation steps,etc.Therefore,it is of great significance to promote the rapid development of new sample pretreatment methods.An overview on the sample pretreatment methods for cosmetic samples analysis in the past five years is provided in this paper.The sample pretreatment methods which are placed special emphasis on in this review are phase separation methods,mainly including solid phase extraction,solid phase microextraction and liquid phase microextraction,field assisted methods including ultrasound-assisted,microwave-assisted and vortex-assisted extraction,and derivatization methods including post-column and pre-column derivatization.These techniques are used in a vast range of modern extraction process,which are of increasing interest.Finally,the prospect of the development direction of sample pretreatments for cosmetics samples analysis are also put forward.