共查询到20条相似文献,搜索用时 15 毫秒
1.
Marques Lde A Catharino RR Bruns RE Eberlin MN 《Rapid communications in mass spectrometry : RCM》2006,20(24):3654-3658
A fast procedure to classify perfumes and identify counterfeit samples is described. Dilution of a few microL of the sample in a 1:1 methanol/water solution is followed by detection of its major polar components via direct infusion electrospray ionization mass spectrometry (ESI-MS) in the positive ion mode. As proof-of-principle cases, three famous brands of perfumes were used. The ESI+-MS fingerprints of authentic samples were very characteristic, showing distinctive sets of polar markers for each sample. Principal component analysis (PCA) placed samples of the three perfume brands in well-defined groups. Counterfeit samples were also clearly detected owing to contrasting ESI-MS fingerprints, with PCA placing these samples far away from the authentic samples. 相似文献
2.
Authentic samples of whisky produced in Scotland and USA and counterfeit whisky samples commercialized in Brazil have been directly submitted to electrospray ionization mass spectrometry (ESI-MS) analysis in both the negative and positive ion modes to assess the potential of this technique for simple and rapid quality control and proof of authenticity of whisky samples. ESI in the negative ion mode yields the most characteristic whisky fingerprinting mass spectra in just a few seconds by direct infusion of the samples, detecting the most polar or acidic components of each sample in their deprotonated anionic forms. No pre-treatment of the sample, such as extraction or derivatization or even dilution, is required. The analysis of the ESI(-)-MS data both by simple visual inspection but more particularly by chemometric data treatment enables separation of the whisky samples into three unequivocally distinct groups: Scotch, American and counterfeit whisky, whereas single malt and blended Scotch whiskies are also distinguished to some extent. As indicated by ESI-MS/MS analysis, the diagnostic anions are simple sugars, disaccharides and phenolic compounds. Direct infusion ESI-MS therefore provides immediate chemical fingerprinting of whisky samples for type, origin and quality control, as demonstrated herein for American, Scottish and counterfeit samples, whereas ESI-MS/MS analysis of diagnostic ions adds a second dimension of fingerprinting characterization when improved selectivity is desired. 相似文献
3.
Romão W Lalli PM Franco MF Sanvido G Schwab NV Lanaro R Costa JL Sabino BD Bueno MI de Sa GF Daroda RJ de Souza V Eberlin MN 《Analytical and bioanalytical chemistry》2011,400(9):3053-3064
Meta-chlorophenylpiperazine (m-CPP) is a new illicit drug that has been sold as ecstasy tablets. Easy ambient sonic-spray ionization mass spectrometry (EASI-MS) and X-ray fluorescence spectrometry (XRF) are shown to provide relatively simple and selective screening tools to distinguish m-CPP tablets from tablets containing amphetamines (mainly 3,4-methylenedioxymethamphetamine (MDMA)). EASI-MS detects the active ingredients in their protonated forms: [m-CPP + H](+) of m/z 197, [MDMA + H](+) of m/z 194, and [2MDMA + HCl + H](+) of m/z 423 and other ions from excipients directly on the tablet surface, providing distinct chemical fingerprints. XRF identifies Cl, K, Ca, Fe, and Cu as inorganic ingredients present in the m-CPP tablets. In contrast, higher Cl concentrations and a more diverse set of elements (P, Cl, Ca, Fe, Cu, Zn, Pt, V, Hf, Ti, Pt, and Zr) were found in MDMA tablets. Principal component analysis applied to XRF data arranged samples in three groups: m-CPP tablets (four samples), MDMA tablets (twenty three samples), and tablets with no active ingredients (three samples). The EASI-MS and XRF techniques were also evaluated to quantify m-CPP in ecstasy tablets, with concentrations ranging from 4 to 40 mg of m-CPP per tablets. The m-CPP could only be differentiated from its isomers (o-CPP and for the three isomers p-CPP) by traveling wave ion mobility mass spectrometry and NMR measurements. 相似文献
4.
Alberici LC Oliveira HC Catharino RR Vercesi AE Eberlin MN Alberici RM 《Analytical and bioanalytical chemistry》2011,401(5):1655-1663
Easy ambient sonic-spray ionization mass spectrometry (EASI-MS) was used to interrogate the hepatic lipid profiles of hypertriglyceridemic
and control normotriglyceridemic mice. The analyses of ex vivo complex lipid mixtures were made directly with EASI-MS without
accompanying separation steps. Intense ions for phosphatidylcholines and triacylglycerols were observed in the positive ion
mode whereas the spectra in the negative ion mode provided profiles of phosphatidylethanolamines and phosphatidylinositol.
EASI-MS was coupled to high-performance thin-layer chromatography for analysis of free fatty acids. Fourier transform–ion
cyclotron resonance–mass spectrometry was also employed to confirm the identity of the detected lipids. We demonstrated higher
incorporation of oleic acid in phosphatidylcholine and triacylglycerol composition, higher relative abundance of arachidonic
acid containing phosphatidylinositol, and overall distinct free fatty acid profile in the livers of genetic hypertriglyceridemic
mice. We propose that these alterations in liver lipid composition are related to the higher tissue and body metabolic rates
described in these hypertriglyceridemic mice. 相似文献
5.
Barbara Pacholczyk-Sienicka Grzegorz Ciepielowski ukasz Albrecht 《Molecules (Basel, Switzerland)》2021,26(11)
The manufacture of counterfeit goods is one of the world’s largest underground businesses and is rapidly growing. Counterfeits can lead not only to the loss of profit for honest producers but also have a negative impact on consumers who pay excessive prices for poor quality goods that may result in health or safety problems. The perfume industry is constantly vulnerable to counterfeits, particularly in the fast developing market of “smell-alike” designer-inspired perfumes because these prompt the identification of the methods that classify their quality. In this paper, the application of proton nuclear magnetic resonance (1H NMR) spectroscopy is employed for the first time to authenticate perfumery products. The molecular composition of several types of authentic brand fragrances for women was compared with cheap inspired equivalents and fakes. Our approach offers the prospect of a fast and simple method for detecting counterfeit perfumes using 1H NMR spectroscopy. 相似文献
6.
Rapid classification of perfumes by extractive electrospray ionization mass spectrometry (EESI-MS) 总被引:1,自引:0,他引:1
Chingin K Gamez G Chen H Zhu L Zenobi R 《Rapid communications in mass spectrometry : RCM》2008,22(13):2009-2014
Extractive electrospray ionization mass spectrometry (EESI-MS) was applied to rapid fingerprinting of various perfumes for quality classification. Unique EESI-MS fingerprints of ten famous brands were obtained. This technique was shown to be applicable to rapid forgery detection on the example of an authentic and a counterfeit 'Miss Dior' fragrance by Christian Dior. We believe that the high throughput and simplicity of this sample-preparation-free method can be advantageous in the perfume industry, for instance when applied to online quality control. 相似文献
7.
8.
建立了气相色谱-质谱同时检测化妆品及香精中27种香料的方法。采用甲醇作为提取溶剂,经弱极性毛细管柱分离,用气相色谱-质谱检测,离子源为电子轰击离子(EI)源。该方法对麝香二甲苯、羟基香茅醛和羟异己基3-环己烯基甲醛的检出限分别为1.2、15和15 mg/kg,其余香料的检出限为3.0 mg/kg。27种香料在相应的线性范围内线性关系良好,相关系数均大于等于0.996。在3个加标浓度下,麝香二甲苯的回收率为73.3%~76.1%,其余为81.5%~118%,相对标准偏差小于10%。采用建立的方法对69份香精或标示含香料化妆品进行检测,全部样品都检测出含有一种或多种香料。该方法适用于化妆品及香精中27种香料的测定。 相似文献
9.
Nørgaard AW Vaz BG Lauritsen FR Eberlin MN 《Rapid communications in mass spectrometry : RCM》2010,24(23):3441-3446
The progress of an on-surface polymerization process involving alkyl and perfluoroalkyl silanes and siloxanes was monitored in real-time via easy ambient sonic spray ionization mass spectrometry (EASI-MS). When sprayed on surfaces, the organosilicon compounds present in commercially available nanofilm products (NFPs) react by condensation to form a polymeric coating. A NFP for coating of floor materials (NFP-1) and a second NFP for coating tiles and ceramics (NFP-2) were applied to glass, filter paper or cotton surfaces and the progress of the polymerization was monitored by slowly scanning the surface. Via EASI(+)-MS monitoring, significant changes in the composition of hydrolysates and condensates of 1H,1H,2H,2H-perfluorooctyl triisopropoxysilane (NFP-1) and hexadecyl triethoxysilane (NFP-2) were observed over time. The abundances of the hydrolyzed species decreased compared with those of the non-hydrolysed species for both NFP-1 and NFP-2 and the heavier oligomers became relatively more abundant over a period of 15-20 min. A similar tendency favouring the heavier oligomers was observed via EASI(-)-MS. This work illustrates the potential of ambient mass spectrometry for the direct monitoring of polymerization reactions on surfaces. 相似文献
10.
Hsu HJ Oung JN Kuo TL Wu SH Shiea J 《Rapid communications in mass spectrometry : RCM》2007,21(3):375-384
We describe the use of electrospray-assisted pyrolysis ionization/mass spectrometry (ESA-Py/MS) to selectively ionize trace polar compounds that coexist with large amounts of nonpolar hydrocarbons in crude oil, amber, humic substances, and rubber samples. Samples of different origins are distinguished rapidly by their positive ion ESA-Py mass spectra without prior separation or chemical pretreatment. During ESA-Py analysis, the samples in their solid or liquid states were pyrolyzed at 590, 630 or 940 degrees C using a commercial Curie-point pyrolysis probe. The gaseous pyrolysates were transferred into a glass reaction cell. The polar compounds (M) in the pyrolysates were then ionized by electrospray ionization (ESI), yielding protonated molecules (MH+). Although the major components of the pyrolysates are nonpolar hydrocarbons, their lack of functional groups that can receive a proton in the ESA-Py source results in no hydrocarbon ion signals being produced; thus, the positive ions detected in ESA-Py mass spectra all result from trace polar components in the pyrolysates. 相似文献
11.
Marina López-Nogueroles Alberto ChisvertAmparo Salvador 《Journal of chromatography. A》2010,1217(18):3150-3160
A chemometric treatment of the data obtained by gas chromatography (GC) with flame ionization detector (FID) has been proposed to study the maceration time involved in perfumes manufacture with the final purpose of reducing this time but preserving the organoleptic characteristics of the perfume that is being elaborated. In this sense, GC–FID chromatograms were used as a fingerprint of perfume samples subjected to different maceration times, and data were treated by linear discriminant analysis (LDA), by comparing to a set of samples known to be macerated or not, which were used as calibration objects. The GC–FID methodology combined with the treatment of data by LDA has been applied successfully to seven different perfumes. The constructed LDA models exhibited excellent Wilks’ lambdas (0.013–0.118, depending on the perfume), and up to a reduction of 57% has been achieved with respect to the maceration time initially established. 相似文献
12.
Mondello L Casillia A Tranchida PQ Dugo G Dugo P 《Journal of chromatography. A》2005,1067(1-2):235-243
Single column gas chromatography (GC) in combination with a flame ionization detector (FID) and/or a mass spectrometer is routinely employed in the determination of perfume profiles. The latter are to be considered medium to highly complex matrices and, as such, can only be partially separated even on long capillaries. Inevitably, several monodimensional peaks are the result of two or more overlapping components, often hindering reliable identification and quantitation. The present investigation is based on the use of a comprehensive GC (GC x GC) method, in vacuum outlet conditions, for the near to complete resolution of a complex perfume sample. A rapid scanning quadrupole mass spectrometry (qMS) system, employed for the assignment of GC x GC peaks, supplied high quality mass spectra. The validity of the three-dimensional (3D) GC x GC-qMS application was measured and compared to that of GC-qMS analysis on the same matrix. Peak identification, in all applications, was achieved through MS spectra library matching and the interactive use of linear retention indices (LRI). 相似文献
13.
Balázs Vajna Attila Farkas Hajnalka Pataki Zsolt Zsigmond Tamás Igricz György Marosi 《Analytica chimica acta》2012
Chemical imaging is a rapidly emerging analytical method in pharmaceutical technology. Due to the numerous chemometric solutions available, characterization of pharmaceutical samples with unknown components present has also become possible. This study compares the performance of current state-of-the-art curve resolution methods (multivariate curve resolution-alternating least squares, positive matrix factorization, simplex identification via split augmented Lagrangian and self-modelling mixture analysis) in the estimation of pure component spectra from Raman maps of differently manufactured pharmaceutical tablets. The batches of different technologies differ in the homogeneity level of the active ingredient, thus, the curve resolution methods are tested under different conditions. An empirical approach is shown to determine the number of components present in a sample. The chemometric algorithms are compared regarding the number of detected components, the quality of the resolved spectra and the accuracy of scores (spectral concentrations) compared to those calculated with classical least squares, using the true pure component (reference) spectra. It is demonstrated that using appropriate multivariate methods, Raman chemical imaging can be a useful tool in the non-invasive characterization of unknown (e.g. illegal or counterfeit) pharmaceutical products. 相似文献
14.
Update on solid-phase extraction for the analysis of lipid classes and related compounds 总被引:2,自引:0,他引:2
This article provides information on the different procedures and methodologies developed when solid-phase extraction (SPE) is used for lipid component separation. The analytical systematics, established by different authors and designed to separate groups of compounds and also specific components by using a combination of chromatographic supports and solvents are presented. The review has been divided into three parts, which we consider well defined: edible fats and oils, fatty foods and biological samples. Separations of non-polar and polar lipids is the most extensive systematic, although many other published methods have been established to isolate specific components or a reduced number of components from edible fats and oils, fatty foods or biological samples susceptible to further analysis by other quantitative techniques. 相似文献
15.
Ricci C Nyadong L Yang F Fernandez FM Brown CD Newton PN Kazarian SG 《Analytica chimica acta》2008,623(2):178-186
Pharmaceutical counterfeiting has become a significant public health problem worldwide and new, rapid, user-friendly, reliable and inexpensive methods for drug quality screening are needed. This work illustrates the chemical characterization of genuine and fake artesunate antimalarial tablets by portable Raman spectroscopy and validation by FT-Raman spectroscopy and ambient mass spectrometry. The applicability of a compact and robust portable Raman spectrometer (TruScan™) for the in situ chemical identification of counterfeit tablets is reported. 相似文献
16.
Sacré PY Deconinck E Daszykowski M Courselle P Vancauwenberghe R Chiap P Crommen J De Beer JO 《Analytica chimica acta》2011,(2):224-231
Most of the counterfeit medicines are manufactured in non good manufacturing practices (GMP) conditions by uncontrolled or street laboratories. Their chemical composition and purity of raw materials may, therefore, change in the course of time. The public health problem of counterfeit drugs is mostly due to this qualitative and quantitative variability in their formulation and impurity profiles.In this study, impurity profiles were treated like fingerprints representing the quality of the samples. A total of 73 samples of counterfeit and imitations of Viagra® and 44 samples of counterfeit and imitations of Cialis® were analysed on a HPLC-UV system. A clear distinction has been obtained between genuine and illegal tablets by the mean of a discriminant partial least squares analysis of the log transformed chromatograms. Following exploratory analysis of the data, two classification algorithms were applied and compared. In our study, the k-nearest neighbour classifier offered the best performance in terms of correct classification rate obtained with cross-validation and during external validation. For Viagra®, both cross-validation and external validation sets returned a 100% correct classification rate. For Cialis® 92.3% and 100% correct classification rates were obtained from cross-validation and external validation, respectively. 相似文献
17.
Essential plants, due to their long presence in human history, their status in culinary arts, their use in medicine and perfume manufacture, belong to frequently examined stock materials in scientific and industrial laboratories. Because of a large number of freshly cut, dried or frozen plant samples requiring the determination of essential oil amount and composition, a fast, safe, simple, efficient and highly automatic sample preparation method is needed.Five sample preparation methods (steam distillation, extraction in the Soxhlet apparatus, supercritical fluid extraction, solid phase microextraction and pressurized liquid extraction) used for the isolation of aroma-active components from Thymus vulgaris L. are compared in the paper. The methods are mainly discussed with regard to the recovery of components which typically exist in essential oil isolated by steam distillation.According to the obtained data, PLE is the most efficient sample preparation method in determining the essential oil from the thyme herb. Although co-extraction of non-volatile ingredients is the main drawback of this method, it is characterized by the highest yield of essential oil components and the shortest extraction time required. Moreover, the relative peak amounts of essential components revealed by PLE are comparable with those obtained by steam distillation, which is recognized as standard sample preparation method for the analysis of essential oils in aromatic plants. 相似文献
18.
《Trends in analytical chemistry : TRAC》2002,21(9-10):698-708
Gas chromatography (GC) and mass spectrometry (MS) are by far the most important analytical techniques in the perfume industry. Both perfume houses (the suppliers) and the home and personal-care companies (the clients) rely primarily on GC and GC-MS for unraveling the composition of perfumes (i.e. perfume formulation), quality control, competitor analysis and trace analysis on substrates and in the headspace. State-of-the-art perfume formulation is based on perfume-specific Kovats Index (KI) and MS databases. By applying FID (flame-ionization detector) response-correction factors, the accuracy of the perfume-formulation process can be further improved. Because of the complexity of perfumes, use is made of GC columns and conditions that offer maximum resolution rather than minimum analysis time. Mass-spectral deconvolution tools can be very useful in identifying perfume ingredients from GC-MS data in cases of co-elution or strong matrix interference. By applying the MS detector in the selected ion monitoring (SIM) mode, GC-MS is very suitable for trace analysis of perfume ingredients, thus enabling the study of perfume efficacy during use of home and personal-care products. Recent developments in the field of comprehensive GC (i.e. GC×GC) also seem very promising for perfume analysis. 相似文献
19.
The application of simplex optimization to the qualitative and quantitative evaluation of chromatograms of complex mixtures is outlined. The chromatogram is considered as a linear combination of pure component chromatograms (assuming no interactions are present); if suitable components are selected and the coefficients of the linear combination are properly evaluated, the experimental chromatogram can be reproduced numerically. The simplex method is then used to evaluate the solution with minimal error. The quantitation of polychlorobiphenyls from Aroclor mixtures in marine sediments and fish, and the identification of essential oils in a perfume base extract are outlined. Errors of ≤19% (25% in environmental samples) between the experimental and reconstructed chromatograms were achieved. 相似文献
20.
A novel two-dimensional reversed-phase liquid chromatography/hydrophilic interaction chromatography (2D-RPLC/HILIC) system is developed with the introduction of the click beta-cyclodextrin (beta-CD) stationary phase. The offline system shows excellent abilities for the separation of polar and medium-polarity components in traditional Chinese medicine (TCM). It facilitates us not only to separate components that cannot be resolved by uni-dimensional chromatography, but also to achieve much more efficient detection of components with low abundance. The orthogonality of this new system is excellent. A simple geometric approach is developed to characterize the practical orthogonality of 2D-LC in the analysis of complex unknown samples. The mathematical characterization results are in good accordance with the experimental findings, and both demonstrate that the proposed 2D-RPLC/HILIC system is a powerful tool for the separation of polar and medium-polarity complex samples. This system may have a great potential for the separation of peptides and metabolomic compounds with similar polarity. 相似文献