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PubMed1996

Preconcentration and determination of Sn- and Pb-organic species in environmental samples by SPME and GC-AED.

A new sample preparation and preconcentration technique - solid phase microextraction (SPME) - is reported for the application of several tinorganic compounds and tetrabutyllead in aqueous samples. The solvent-free procedure is rapid in comparison with liquid-liquid extraction or SFE but also sensitive. Analytical variables of the extraction such as adsorption and desorption time, stirring rate and temperature has been investigated. The determination has been performed by GC coupled with atomic emission detection (AED). After optimization of the conditions of SPME a calibration was realized on the basis of a multicomponent standard solution, prepared by ethylation of organotin salts directly in the sample using sodium tetraethylborate (NaBEt(4)) without prior separation of the analytes from the matrix. The method permits preconcentration. Values of about 10 can be reached. A detection limit of 0.09 pg Sn and 0.08 pg Pb can be achieved under optimized conditions. The proposed procedure has been successfully applied to the analysis of organotin compounds in various slurry samples.

Journal Article↗
PubMed2000

Solid-phase microextraction: a promising technique for sample preparation in environmental analysis.

Solid-phase microextraction (SPME) is a simple and effective adsorption and desorption technique, which eliminates the need for solvents or complicated apparatus, for concentrating volatile or nonvolatile compounds in liquid samples or headspace. SPME is compatible with analyte separation and detection by gas chromatography and high-performance liquid chromatography, and provides linear results for wide concentrations of analytes. By controlling the polarity and thickness of the coating on the fibre, maintaining consistent sampling time, and adjusting other extraction parameters, an analyst can ensure highly consistent, quantifiable results for low concentration analytes. To date, about 400 articles on SPME have been published in different fields, including environment (water, soil, air), food, natural products, pharmaceuticals, biology, toxicology, forensics and theory. As the scope of SPME grew, new improvements were made with the appearance of new coatings that allowed an increase in the specificity of this extraction technique. The key part of the SPME fibre is of course the fibre coating. At the moment, 27 variations of fibre coating and size are available. Among the newest are a fibre assembly with a dual coating of divinylbenzene and Carboxen suspended in poly(dimethylsiloxane), and a series of 23 gauge fibres intended for specific septumless injection system. The growth of SPME is also reflected in the expanding number of the accessories that make the technology even easier to use Also available is a portable field sampler which is a self-contained unit that stores the SPME fibre after sampling and during the shipment to the laboratory. Several scientific publications show the results obtained in inter-laboratory validation studies in which SPME was applied to determine the presence of different organic compounds at ppt levels, which demonstrates the reliability of this extraction technique for quantitative analysis.

Chromatography, Gas↗
PubMed2003

Compound-specific carbon isotope analysis of volatile organic compounds in the low-microgram per liter range.

Compound-specific carbon isotope analysis (CSIA) has become an important tool in biological, archeological, and geological studies as well as in forensics, food sciences, and organic chemistry. If sensitivity could be enhanced, CSIA would further have an improved potential for environmental applications such as, for example, in situ remediation studies to assess contaminated environments, identification of pollutant degradation pathways and kinetics, distinction between degradation/formation mechanisms, or, verification of contaminant sources. With this goal in mind, we have developed methods to determine delta13C values of commonly reported groundwater contaminants in low-microgram per liter concentrations. Several injection and preconcentration techniques were evaluated for this purpose, i.e., on-column injection, split/ splitless injection, solid-phase microextraction (SPME), and purge and trap (P&T) in combination with gas chromatography-isotope ratio mass spectrometry. The delta13C values of the target compounds were determined by liquid injections of the analytes dissolved in diethyl ether or, in the case of P&T and SPME, by extraction from water spiked with the analytes. P&T extraction was the most efficient preconcentration technique reaching method detection limits (MDLs) from 0.25 to 5.0 microg/L. These are the lowest MDLs reported so far for continuous-flow isotope ratio determinations, using a commercially available and fully automated system. Isotopic fractionation resulting from preconcentration and injection was investigated and quantified for the priority groundwater pollutants methyl tert-butyl ether (MTBE), chloroform, tetrachloromethane, chlorinated ethylenes, benzene, and toluene. The isotopic fractionations caused by the extraction techniques were small but highly reproducible and could therefore be corrected for. P&T was characterized by a higher reproducibility and smaller isotopic fractionations than SPME. Among the liquid injection techniques, cold on-column injection resulted in slightly better precision compared to split/splitless injection. However, the MDLs determined for liquid injections were 4-6 orders of magnitude higher (i.e., 9.5-2800 mg/L) than for P&T and SPME. Since both of the latter methods are solventless, a better chromatographic resolution was obtained than for the liquid injection techniques. The P&T and SPME methods described here are also applicable for CSIA of D/H ratios, which require 10-20 times higher analyte concentrations than 13C/12C analysis. Finally, the applicability of the described methods is demonstrated for pollutant concentrations of only 5-60 microg/L in environmental samples.

Journal Article↗
PubMed1999

[Estimation of the octanol-water partition coefficients of PAHs by solid-phase microextraction].

Eleven PAHs were analyzed by solid-phase microextraction-gas chromatography/ion trap detector and their partition coefficients were obtained at equilibrium. When the polymer coating of the fiber may be viewed as one kind of organic solvent, the linear free energy relationship between the polydimethylsiloxane-water partition coefficient (Ksw) and octanol-water partition coefficient (Kow) was established by solid-phase microextraction, which was log Ksw = 0.9318 log Kow-0.2056 with good correlation coefficient 0.9504. The linear equation may be used to estimate the octanol-water partition coefficient of other PAHs and similar H acceptors compounds. Being compared with Leo's method which was based on the additive-constitutive nature of the partition coefficient, the solid-phase microextraction method may distinguish efficiently Kow of the isomer.

Chromatography, Gas↗
PubMedDate not supplied

Determination of thiabendazole in orange juice and rind by liquid chromatography with fluorescence detection and confirmation by gas chromatography/mass spectrometry after extraction by matrix solid-phase dispersion.

A method was developed for the determination of thiabendazole (TBZ) in orange juice and rind based on matrix solid-phase dispersion (MSPD). TBZ was extracted with ethyl acetate and the extract was subsequently cleaned up on a solid-phase extraction column. Fungicide residues were determined by liquid chromatography with fluorescence detection. Recoveries through the method ranged from 87 to 97% with relative standard deviations < or = 11%. The detection and quantitation limits were 0.15 and 0.50 microg/kg, respectively. The confirmation of TBZ residues in positive samples was performed by solid-phase microextraction followed by gas chromatography with mass spectrometric detection using selected ion monitoring. The developed method was applied to determine TBZ levels in commercial orange juices and in juice and rind of fresh oranges. The influence of storage and washing of fruits on TBZ residues was also studied.

Beverages↗
PubMed2006

Determination of n-octanol-water partition coefficients by hollow-fiber membrane solvent microextraction coupled with HPLC.

A novel direct method has been developed for determination of n-octanol-water partition coefficients by hollow-fiber membrane solvent microextraction (HFMSME) combined with high-performance liquid chromatography (HPLC). The compound of interest is dissolved in water with sonication and a hollow fiber containing octanol inside is placed in the sample solution to perform microextraction. After microextraction the concentrations in both the aqueous and n-octanol phases are analyzed by HPLC with UV detection. The method was evaluated with ten reference compounds and shown to be suitable for determination of the partition coefficients of organic compounds accurately, cheaply, simply, and quickly. Previously unknown n-octanol-water partition coefficients have been obtained for other compounds by use of the hollow-fiber membrane solvent-microextraction technique.

1-Octanol↗
PubMed2004

Highly sensitive analysis of multiple pesticides in foods combining solid-phase microextraction, capillary electrophoresis-mass spectrometry, and chemometrics.

A highly sensitive procedure to detect multiple pesticides at trace levels in foods is presented. Initially a comparative study between capillary electrophoresis (CE)-UV and CE-mass spectrometry (MS) is carried out analyzing five pesticides not studied up to now (pyrimethanil, pyrifenox, cyprodinil, cyromazine, and pirimicarb). The comparison between CE-UV and CE-MS is established in terms of separation efficiency, speed of analysis, reproducibility, and sensitivity. A good separation of these compounds is achieved by both techniques using a volatile aqueous buffer containing 0.3 M ammonium acetate/acetic acid at pH 4. Time analysis reproducibility is studied for the same day (n = 5) and three different days (n = 15), showing no significant differences between CE-UV and CE-MS. The study on peak areas reproducibility shows a slightly worse reproducibility for CE-MS compared with CE-UV. The best limit of detection (LOD) that can be achieved for these pesticides using CE-UV was 0.6 microg/mL. CE-MS provides LODs one order of magnitude better than CE-UV. Chemometrics are used to optimize the multiple parameters that play a role in solid-phase microextraction (SPME) and CE-MS analysis (e.g., extraction and desorption times, nebulizer pressure, dry gas flow, dry gas temperature, percentage of organic solvent and acid in the sheath liquid, etc.). The combined use of chemometrics and SPME-CE-MS clearly improves the LODs that can be achieved allowing the detection of pesticides at concentrations down to 15 ng/mL. The usefulness of this approach is demonstrated detecting multiple pesticides in different food samples as grapes and orange juice in a single run. The concentrations detected are below the maximum residue limits (MRLs) permitted for these pesticides in foods corroborating the value of our approach. This work demonstrates, to our knowledge for the first time, the good possibilities of the combined use of SPME-CE-MS and chemometrics.

Absorption↗
PubMed2006

Environmental and biological monitoring of benzene exposure in a cohort of Italian taxi drivers.

An integrated approach based on ambient and biological monitoring, the latter including both biomarkers of exposure and susceptibility, was applied to characterize benzene exposure in a group of 37 taxi drivers of the city of Parma (Italy). Airborne benzene concentrations were assessed by 24 h personal sampling and work-shift sampling inside the taxicab using passive samplers (Radiello). Benzene metabolites, trans,trans-muconic acid (t,t-MA) and S-phenylmercapturic acid (S-PMA), and urinary cotinine as biomarker of smoking habits were measured by isotopic dilution liquid chromatography tandem mass spectrometry in both pre-shift (PS) and end-of-shift (EOS) samples. Urinary benzene (U-B) levels were determined by solid-phase microextraction gas chromatography-mass spectrometry in EOS samples. Relevant polymorphisms of microsomal epoxide hydrolase, NAD(P)H:quinone oxidoreductase, glutathione S-transferases M1-1 (GSTM1), T1-1, and A1 were characterized by PCR-based methods. Mean airborne benzene concentration was 5.85 +/- 1.65 microg/m3, as assessed by 24 h personal sampling integrating for work-shift, indoor or general environment activities. Significantly, higher benzene concentrations were detected in the taxicab during the work-shift (7.71 +/- 1.95 microg/m3, p < 0.005). Smokers eliminated significantly higher concentrations of U-B and S-PMA than non-smokers in EOS samples [geometric mean (geometric S.D.): 2.58 (4.23) versus 0.44 (1.79) microg/l for U-B; 3.79 (1.50) versus 2.14 (1.87) microg/gcreat. for S-PMA, p < 0.002]. Within smokers, S-PMA concentrations significantly increased at the end of the work-shift compared to pre-shift values (p < 0.05). t,t-MA showed a similar behaviour, although differences were not significant. In the narrow range examined, no correlation was observed between air benzene concentration and urinary biomarkers. All benzene biomarkers but EOS t,t-MA were correlated with U-cotinine (p < 0.05). GSTM1 polymorphism significantly modulated S-PMA excretion, as subjects bearing the GSTM1pos genotype [3.61 (1.15) microg/gcreat.] excreted significantly higher S-PMA concentrations than GSTM1null subjects [2.19 (1.18) microg/gcreat., p < 0.05].

Acetylcysteine↗
PubMed2002

Miniaturized solid-phase extraction as a sample preparation technique for the determination of phthalates in water.

Miniaturized solid-phase extraction (SPE) has been developed and successfully employed for the determination of organic species in water samples by liquid chromatography (LC). The method is based on the concept of a microscale extraction technique using a fused-silica capillary column for gas chromatography (GC), so-called in-tube solid-phase microextraction (SPME). The extraction conditions, such as the extraction time and flow-rate for the extraction and desorption process, were investigated as well as the effect of the internal structure of the extraction capillary on the efficiency. By inserting a stainless steel wire into the extraction capillary to reduce the internal volume of the capillary with the same surface area of the coating, an improved extraction and pre-concentration effects were obtained. Further pre-concentration was accomplished by the extraction device with a novel fiber-in-tube configuration. The direct coupling of the extraction method with a LC system has made it possible to determine low levels of phthalates in water samples without high consumption of organic solvents. The system developed must have potential applications for the analysis of environmental and biological samples in aqueous sample matrices.

Capillary Action↗
PubMed2006

Liquid chromatography electrospray tandem mass spectrometric and desorption electrospray ionization tandem mass spectrometric analysis of chemical warfare agents in office media typically collected during a forensic investigation.

Most prior analytical studies have dealt with the determination of chemical warfare agents in environmental or biological matrices that would typically be collected following battlefield use or in support of the Chemical Weapons Convention. These methods may be useful for some investigations, but may not be practical for indoor forensic investigations where chemical warfare agent use is suspected. There is a need for analytical methods for chemical warfare agent identification in office media, including flooring, wall surfaces, office fabrics and paper products, which would typically be collected in an office environment during forensic investigations. During this study, typical office environment media were spiked at the 4-20microg/g level with either a complex munitions grade sample of tabun (GA) or with a standard containing the three nerve agents, sarin (GB), cyclohexyl methylphosphonofluoridate (GF), soman (GD) and the nerve agent simulant, triethyl phosphate (TEP), to evaluate the potentials of liquid chromatography electrospray ionization mass spectrometry (LC-ESI-MS) and liquid chromatography electrospray ionization tandem mass spectrometry (LC-ESI-MS/MS) for forensic purposes. An emerging technique, desorption electrospray ionization (DESI-MS/MS), was also investigated for the direct determination of TEP, GB and GD sampled onto solid phase microextraction (SPME) fibers exposed to spiked office media. The spiked chemical warfare agents were recovered with varying efficiencies during this study, but in all cases sufficient chemical warfare agent was recovered for mass spectrometric identification purposes. Full high resolution mass spectra were acquired for all the chemical warfare agents in the continuum mode, which typically resulted in mass measurement errors of 0.001Da or less.

Central Nervous System Agents↗
PubMed2004

Automated headspace solid-phase dynamic extraction to analyse the volatile fraction of food matrices.

High concentration capacity headspace techniques (headspace solid-phase microextraction (HS-SPME) and headspace sorptive extraction (HSSE)) are a bridge between static and dynamic headspace, since they give high concentration factors as does dynamic headspace (D-HS), and are as easy to apply and as reproducible as static headspace (S-HS). In 2000, Chromtech (Idstein, Germany) introduced an inside-needle technique for vapour and liquid sampling, solid-phase dynamic extraction (SPDE), also known as "the magic needle". In SPDE, analytes are concentrated on a 50 microm film of polydimethylsiloxane (PDMS) and activated carbon (10%) coated onto the inside wall of the stainless steel needle (5 cm) of a 2.5 ml gas tight syringe. When SPDE is used for headspace sampling (HS-SPDE), a fixed volume of the headspace of the sample under investigation is sucked up an appropriate number of times with the gas tight syringe and an analyte amount suitable for a reliable GC or GC-MS analysis accumulates in the polymer coating the needle wall. This article describes the preliminary results of both a study on the optimisation of sampling parameters conditioning HS-SPDE recovery, through the analysis of a standard mixture of highly volatile compounds (beta-pinene, isoamyl acetate and linalool) and of the HS-SPDE-GC-MS analyses of aromatic plants and food matrices. This study shows that HS-SPDE is a successful technique for HS-sampling with high concentration capability, good repeatability and intermediate precision, also when it is compared to HS-SPME.

Food Analysis↗
PubMed2000

Solid-phase extraction of phenols.

Sample preparation for phenol analysis using solid-phase extraction (SPE) is reviewed. The scope of the review has been restricted to the literature dealing with the analysis of phenols as the main objective. The use, advantages and disadvantages of silica sorbents, polymeric, functionalized, carbon-based and mixed available sorbents, when applied to the separation and preconcentration of phenols, as well as the available experimental devices, are discussed. Other aspects such as phenol derivatisation prior to SPE, solid-phase microextraction, matrix effects and the storage of phenols in SPE cartridges, have been also discussed.

Chromatography, Liquid↗
PubMed2006

Solid-phase microextraction method for carbon isotopic analysis of volatile carboxylic acids in human plasma by gas chromatography/combustion/isotope ratio mass spectrometry.

A new analytical method is described for the determination of the physiological concentration and low-level enrichment of (13)C-short-chain volatile organic acids (SCVAs) (e.g. (13)C-acetate and (13)C-butyrate) in human plasma. This two-step method involves solid-phase microextraction (SPME) coupled to gas chromatography/combustion/isotope ratio mass spectrometry (GC/C/IRMS) without any organic solvents or derivatizing agents. Two SCVA extraction methods were compared using a carboxen/polydimethylsiloxane fiber: headspace sampling (HS) and liquid sampling (LS) SPME. The influences of extraction temperature and time were tested to optimize the adsorption of SCVAs onto the fiber. The comparison of the peak area responses of the acids in the two adsorption methods showed better sensitivity in the human physiological concentration range in the LS mode than in the HS mode. The accuracy of isotopic enrichment measurement was determined using plasma spiked with (13)C-acetate and (13)C-butyrate solution from 0 to 1 mol percent excess (MPE). The linearity and repeatability (RSD < 5%) were measured in LS mode. Plasma SCVA concentrations were also determined relative to 3-methylvalerate (internal standard). Linearity and repeatability were observed from 0 to 400 microM for acetate, from 0 to 20 microM for propionate, and from 0 to 10 microM for butyrate. This method was also used to determine plasma acetate production obtained from lactulose (an undigestible disaccharide) fermentation in one healthy volunteer over 3 h. The acetate concentration increased twofold, 2 h after oral lactulose intake. These results are in agreement with the data obtained by GC/MS in healthy volunteers and obese adults following a lactulose intake by using higher amounts of labelled tracers.SPME coupled with GC/C/IRMS can be used to analyze (13)C-SCVAs at low enrichment (<0.5 MPE) within the physiological concentration measured in human plasma.

Algorithms↗
PubMed2000

The use of solid-phase microextraction--gas chromatography in forensic analysis.

A thorough review of the application of solid-phase microextraction (SPME) combined with gas chromatography for the analysis of forensic specimens is presented, including experimental results for several recent applications. The SPME applications covered in this comprehensive review include ignitable liquid residues (also referred to as accelerants), explosive traces, drugs and poisons from biological specimens, and other forensic applications. Recently developed SPME methods are also presented, including the analysis of ignitable liquid residues on human skin, odor signatures, and several drug applications such as free-fraction antipsychotic drug levels, blood alcohol casework, drink-tampering analysis, and gamma-hydroxybutyrate identification without the need for derivatization. SPME is shown to be an inexpensive, rapid, and sensitive method for the analysis of a variety of forensic specimens.

Blood Chemical Analysis↗
PubMed2005

Automated dynamic liquid-liquid-liquid microextraction followed by high-performance liquid chromatography-ultraviolet detection for the determination of phenoxy acid herbicides in environmental waters.

Automated dynamic liquid-liquid-liquid microextraction (D-LLLME) controlled by a programmable syringe pump and combined with HPLC-UV was investigated for the extraction and determination of 5 phenoxy acid herbicides in aqueous samples. In the extraction procedure, the acceptor phase was repeatedly withdrawn into and discharged from the hollow fiber by the syringe pump. The repetitive movement of acceptor phase into and out of the hollow fiber channel facilitated the transfer of analytes into donor phase, from the organic phase held in the pore of the fiber. Parameters such as the organic solvent, concentrations of the donor and acceptor phases, plunger movement pattern, speed of agitation and ionic strength of donor phase were evaluated. Good linearity of analytes was achieved in the range of 0.5-500 ng/ml with coefficients of determination, r2 > 0.9994. Good repeatabilities of extraction performance were obtained with relative standard deviations lower than 7.5%. The method provided up-to 490-fold enrichment within 13 min. In addition, the limits of detection (LODs) ranged from 0.1 to 0.4 ng/mL (S/N = 3). D-LLLME was successfully applied for the analysis of phenoxy acid herbicides from real environmental water samples.

2,4,5-Trichlorophenoxyacetic Acid↗
PubMed2006

Comparison of the compositional, microbiological, biochemical, and volatile profile characteristics of nine Italian ewes' milk cheeses.

Nine Italian ewes' milk cheeses were compared for compositional, microbiological, biochemical, and volatile profile characteristics. Mean values for the gross composition were rather similar among cheeses. The lowest pH values were found for cheeses that used primary starters. At the end of ripening, cheeses made from raw milk contained >6.0 log10 cfu/g of nonstarter lactic acid bacteria. Several species of lactobacilli were identified, but Lactobacillus plantarum and Lactobacillus paracasei were dominant. Random amplified polymorphic DNA-PCR analysis showed the biodiversity among the strains, and in several cases a relationship with the cheese of provenance. Cheeses differed mainly for secondary proteolysis, as shown by the principal component analysis applied to reversed-phase fast protein liquid chromatography data of the pH 4.6-soluble fractions and by determination of the free AA. A total of 113 volatile components were identified in the Italian Pecorino cheeses by solid-phase microextraction coupled with gas chromatography-mass spectrometry analysis. The volatile profiles of the 9 cheeses differed significantly. Quantitatively, alcohols were the most abundant chemical class for some cheeses, whereas ketones were the most abundant for other cheeses. Esters and carboxylic acids were largely found. Specific volatile components seemed to distinguish specific cheeses.

Amino Acids↗
PubMed2005

Orthogonal array designs for the optimization of liquid-liquid-liquid microextraction of nonsteroidal anti-inflammatory drugs combined with high-performance liquid chromatography-ultraviolet detection.

Orthogonal array designs (OADs) were applied for the first time to optimize liquid-liquid-liquid microextraction (LLLME) conditions for the analysis of three nonsteroidal anti-inflammatory drug residues (2-(4-chlorophenoxy)-2-methylpropionic acid, ketoprofen, and naproxen) in wastewater samples. Six relevant factors were investigated: type of organic solvent, composition of donor phase and acceptor phase, stirring speed, extraction time and salt concentration. In the first stage, mixed-level orthogonal array design, an OA16 (4(1) x 2(12)) matrix was employed to study the effect of six factors, by which the effect of each factor was estimated using individual contributions as response functions. Based on the results of the first stage, 1-octanol was chosen as organic solvent for extraction. The other five factors were selected for further optimization using an OA16 (4(5)) matrix and a 4 x 4 table to locate more exact levels for each variable. The relative standard deviations for the reproducibility of optimized LLLME varied from 6.2 to 7.1%. The coefficients of determination for calibration curves were higher than 0.9950. The method detection limits for drugs spiked in ultrapure water were in the range of 0.03-0.3 ng/mL. The final optimized conditions were applied to the analysis of drug residues in three wastewater samples in Singapore.

Anti-Inflammatory Agents, Non-Steroidal↗
PubMed2006

A high-throughput, fully automated liquid/liquid extraction liquid chromatography/mass spectrometry method for the quantitation of a new investigational drug ABT-869 and its metabolite A-849529 in human plasma samples.

ABT-869 is a novel ATP-competitive inhibitor for all the vascular endothelial growth factor (VEGF) and platelet-derived growth factor (PDGF) receptor tyrosine kinases (RTKs). It is one of the oncology drugs in development at Abbott Laboratories and has great potential for enhanced anti-tumor efficacy as well as activity in a broad range of human cancers. We report here an accurate, precise and rugged liquid chromatography/mass spectrometry (LC/MS/MS) assay for the quantitative measurement of ABT-869 and its acid metabolite A-849529. A fully automated 96-well liquid/liquid extraction method was achieved utilizing a Hamilton liquid handler. The only manual intervention required prior to LC/MS/MS injection is to transfer the 96-well plate to a drying rack to dry the extracts then transfer the plate back to the Hamilton for robotic reconstitution. The linear dynamic ranges were from 1.1 to 598.8 ng/mL for ABT-869 and from 1.1 to 605.8 ng/mL for A-849529. The coefficient of determination (r2) for all analytes was greater than 0.9995. For the drug ABT-869, the intra-assay coefficient of variance (CV) was between 0.4% and 3.7% and the inter-assay CV was between 0.9% and 2.8%. The inter-assay mean accuracy, expressed as percent of theoretical, was between 96.8% and 102.2%. For the metabolite A-849529, the intra-assay CV was between 0.5% and 5.1% and the inter-assay CV was between 0.8% and 4.9%. The inter-assay mean accuracy, expressed as percent of theoretical, was between 96.9% and 100.6%.

Blood Chemical Analysis↗