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1.
Environ Monit Assess ; 196(2): 175, 2024 Jan 19.
Article in English | MEDLINE | ID: mdl-38240934

ABSTRACT

The present study implements a methodology to estimate water quality values using statistical tools and remote sensing techniques in a tropical water body Sanalona. Linear regression models developed by Box-Cox transformations and processed data from LANDSAT-8 imagery (bands) were used to estimate TOC, TDS, and Chl-a of the Sanalona reservoir from 2013 to 2020 at five sampling sites measured every 6 months. A band discriminant analysis was carried out to statistically fit and optimize the proposed algorithms. Coefficients of determination beyond 0.9 were obtained for these water quality parameters (r2TOC = 0.90, r2TDS = 0.95, and r2Chl-a = 0.96). A comparison between the estimated and observed water quality was carried out using different data for validation. The validation of the models showed favorable results with R2TOC = 0.8525, R2TDS = 0.8172, and R2Chl-a = 0.9256. The present study implemented, validated, and compared the results obtained by using an ordered and standardized methodology proposed for the estimation of TOC, TDS, and Chl-a values based on water quality parameters measured in the field and using satellite images.


Subject(s)
Chlorophyll , Remote Sensing Technology , Chlorophyll A/analysis , Chlorophyll/analysis , Mexico , Environmental Monitoring/methods , Water Quality , Algorithms
2.
Anal Bioanal Chem ; 416(1): 255-264, 2024 Jan.
Article in English | MEDLINE | ID: mdl-37924377

ABSTRACT

In this work, a low-cost and eco-friendly paper-based analytical device (PAD) method is described for the determination of phyto-cannabinoids in cannabis and oral fluids based on a simple colorimetric reaction. The PAD was able to distinguish tetrahydrocannabinol (THC)- and cannabidiol (CBD)-rich plant samples by using 4-aminophenol (4-AP) and later on to quantify total phyto-cannabinoid content (THC + CBD + CBN) in plant and oral fluids by using the Fast Corinth V reagent. The chemical and physical properties regarding paper type and reagent concentration in the PAD were optimized to achieve the best analytical performance. After that, analytical features were obtained, including a linear range of 0.01-0.1 mg mL-1, a limit of detection (LOD) of 0.003 mg mL-1, and a suitable precision, expressed as relative standard deviation (RSD) lower than 10%. Furthermore, no significant interferences were observed in colorimetric reactions when tea, herbs, and drug samples were analyzed. Additionally, the PAD proved color stability up to 1 month after the sampling at 25 °C. The developed PAD was suitable for determining total phyto-cannabinoid content in plants and oral fluids, obtaining good results compared to GC-MS. Overall, this method showed good reliability resulting in an operational on-site device for drug monitoring.


Subject(s)
Cannabidiol , Cannabinoids , Cannabis , Cannabinoids/analysis , Dronabinol/analysis , Reproducibility of Results , Cannabis/chemistry , Cannabidiol/analysis
3.
Food Res Int ; 174(Pt 1): 113614, 2023 12.
Article in English | MEDLINE | ID: mdl-37986536

ABSTRACT

Alkaloids are naturally occurring compounds containing basic nitrogen atoms. They are biosynthesized mainly by plants but also by some fungi species. Many alkaloids are toxic to humans and animals, and they have been classified as food contaminants. Among them, ergot, tropane, and pyrrolizidine alkaloids have maximum levels in foods, established by the Commission Regulation (EU) 2023/915. In this study, an analytical method was successfully developed and validated for the simultaneous determination of 42 ergot, tropane, and pyrrolizidine alkaloids and their N-oxides in cereal-based food. The method includes QuEChERS-based extraction followed by liquid chromatography coupled with tandem mass spectrometry. The proposed method was validated providing recoveries ranging from 71 to 119 %, intra- and inter-day precision lower than 19 %, and limits of quantification between 0.5 and 1.0 µg kg-1. Finally, the analysis of reference materials coming from FAPAS proficiency tests demonstrated the suitability for purpose of the methodology (z-scores < 2). Nine cereal-based products samples were analyzed of which ergot alkaloids were detected in two of them, while one sample showed the presence of three pyrrolizidine alkaloids.


Subject(s)
Pyrrolizidine Alkaloids , Tandem Mass Spectrometry , Humans , Chromatography, Liquid/methods , Tandem Mass Spectrometry/methods , Pyrrolizidine Alkaloids/analysis , Edible Grain/chemistry , Tropanes/analysis
4.
Mikrochim Acta ; 190(7): 271, 2023 06 23.
Article in English | MEDLINE | ID: mdl-37351649

ABSTRACT

A new concept of paper-based device has been developed combining the advantages of cellulose supports and the rich surface chemistry of metal-organic frameworks (MOFs). The composite, named as NH2-UiO-66@paper, has been developed for the isolation of synthetic cannabinoid receptor agonists (SCRAs) in oral fluids, trying to mimic the interactions of those compounds with the human CB1R and CB2R receptors, mainly governed by hydrogen bonding and π-interactions with serine and histidine residues. MOF selection (UiO-66) and functionalization of the ligand (2-aminoterephthalic acid) has been done according to the following criteria: (i) water stability of the selected MOF, and (ii) promoting appropriate interactions with SCRAs due to the MOF nature. NH2-UiO-66@paper composite has been characterized in depth and the results confirmed that the material is stable at the temperature selected for thermal desorption (230 °C). Furthermore, the developed method provided appropriate precision values (RSD < 12%) and a limit of detection as low as 10 ng using ion mobility spectrometry as analytical technique. Lastly, the method has been successfully applied to the isolation of several synthetic cannabinoids from oral fluids. This method claims to be an interesting approach for expanding the combination of MOFs with sustainable support and represents a promising alternative to sophisticated and non-portable systems due to the negligible sample treatment required and the simplicity of the operation, which can be applied with screening purposes.


Subject(s)
Cannabinoids , Metal-Organic Frameworks , Organometallic Compounds , Phthalic Acids , Humans , Metal-Organic Frameworks/chemistry , Ion Mobility Spectrometry
5.
Anal Chim Acta ; 1246: 340887, 2023 Mar 15.
Article in English | MEDLINE | ID: mdl-36764780

ABSTRACT

In this work, metal-organic frameworks (MOFs) were used for the first time as solid-phase extraction (SPE) sorbents for the isolation of synthetic cannabinoids (SCs) from oral fluids and subsequently quantified by LC-fluorescence detection (FLD). In this context, different MOF families were synthesized and tested under SPE mode. UiO-66 was the family selected, being the amino functionalized (NH2-UiO-66) the best candidate in terms of extraction performance. After the method optimization, several analytical parameters of interest were obtained, reaching limits of detection (LODs) as low as 0.6-0.8 µg L-1 and precision values (expressed as RSD) lower than 10.6%. The developed method was successfully applied to the determination of 8 SCs in different oral fluids at three spiked levels with recoveries between 67 and 114%. This method claims to be a real alternative for screening purposes, being a cost-effective procedure due to the price of the sorbent (<0.5 €/cartridge) and its recyclability (up to 12 uses), among others good features.


Subject(s)
Metal-Organic Frameworks , Organometallic Compounds , Phthalic Acids , Humans , Solid Phase Extraction/methods , Chromatography, High Pressure Liquid/methods
6.
Environ Sci Pollut Res Int ; 29(52): 79478-79496, 2022 Nov.
Article in English | MEDLINE | ID: mdl-35710973

ABSTRACT

The water concentrations of 12 heavy and other metals/metalloids were analyzed seasonally along two horizontal-flow constructed wetlands (CWs) (Tancat Mília-TM and Tancat l'Illa-TLI) located within the Mediterranean Albufera de València Natural Park during 2020-2021. A wide-scope screening of pesticides present in waters was also performed. The two CWs were created to improve water quality and increase biodiversity. They currently receive effluent waters from two different tertiary-treatment wastewater plants, and the water flows along the CWs before being discharged into the main lagoon and a smaller lagoon in TM and TLI, respectively. TLI manages to reduce (Mn) or maintain the concentration of most of the studied elements (Zn, Ni, Hg, Cr, Fe Cd, Cu) at the same level as outside (67%). Only Al, Pb, B, and As remain at a higher concentration. TM also reduces Zn and Cu and keeps the concentration of Cr, Cd, and Hg (representing 42%). Al, Pb, B, and As remain at higher concentrations, as in TLI, but Ni, Fe, and Mn are also at higher concentrations. Although both CWs vary in their ability to remove elements, no risks to human health or the environment have been detected due to the low metal concentration in their outlets, all of them (except Hg) below the legal limits for environmental quality in the European Union. With the detection of 71 compounds in water in each CW area (26 herbicides, 26 insecticides, and 19 fungicides in TLI, and 29 herbicides, 23 insecticides, and 19 fungicides in TM), we also provide evidence of the impact of pesticides, which depends on the application method (helicopter, tractor), originated from areas with high agricultural pressure (chiefly rice crops) on systems (mainly TM) created to preserve biodiversity. Nevertheless, both systems provide crucial environmental services in water quality in this agrolandscape.


Subject(s)
Fungicides, Industrial , Herbicides , Insecticides , Mercury , Metalloids , Metals, Heavy , Pesticides , Water Pollutants, Chemical , Humans , Wetlands , Wastewater , Deuterium Oxide , Cadmium , Lead , Water Pollutants, Chemical/analysis , Metals, Heavy/analysis , Environmental Monitoring/methods
7.
Drug Test Anal ; 14(4): 594-603, 2022 Apr.
Article in English | MEDLINE | ID: mdl-34750997

ABSTRACT

Synthetic cannabinoids are the second largest group of new psychoactive substances reported by the United Nations Office on Drugs and Crime in the last decade and case reports bring attention to its high potency effects and its severe toxicity, including fatalities. Moreover, synthetic cannabinoids are usually entirely metabolized and metabolic pathways for many new generation synthetic cannabinoids are still unknown. In this study, the metabolism of five third generation synthetic cannabinoids was evaluated using zebrafish (Danio rerio) larvae as 24-h in vivo model studied within 5 days after fertilization. The studied synthetic cannabinoids were MMB-CHMICA, ADB-CHMICA, ADB-CHMINACA, MDMB-CHMCZCA, and NNL-3, and the respective metabolites were identified by liquid chromatography-high resolution tandem mass spectrometry. Eleven, six, fourteen, eleven, and four metabolites were identified for MMB-CHMICA, ADB-CHMICA, ADB-CHMINACA, MDMB-CHMCZCA, and NNL-3, respectively, and metabolic pathways have been proposed. The use of zebrafish larvae, with a high degree of physiological and genetic homology to humans, is an emerging tool very useful for the identification of metabolic pathways of psychoactive substances. Results obtained in this study compared well with metabolites obtained previously for the same target molecules or structural analogous after in vitro incubation with human or rat hepatocytes. Thus, potential biomarkers for the evaluated compounds are the O-demethylated metabolite for MMB-CHMICA; the oxidative deamination to hydroxyl metabolite for ADB-CHMICA; hydroxyl metabolites at cyclohexylmethyl, tert-butyl, and indazole moieties for ADB-CHMINACA; hydroxyl metabolites at carbazole core, tert-butyl, or cyclohexylmethyl tail moieties for MDMB-CHMCZCA; and amide hydrolyzed, defluorinated, and dihydroxilated metabolite for NNL-3.


Subject(s)
Cannabinoids , Illicit Drugs , Animals , Cannabinoids/metabolism , Chromatography, Liquid/methods , Illicit Drugs/metabolism , Larva/metabolism , Rats , Zebrafish/metabolism
8.
Talanta ; 238(Pt 1): 122966, 2022 Feb 01.
Article in English | MEDLINE | ID: mdl-34857341

ABSTRACT

In this study, a gas chromatograph (GC) has been coupled to a drift tube ion mobility spectrometer (IMS) in order to develop an analytical procedure for the determination of psychoactive substances in oral fluids. Working parameters, including the GC-IMS interface ones, were adjusted in order to obtain sensitive and robust signals. A volume of 500 µL of oral fluid was extracted with 250 µL chloroform and, after centrifugation, were injected into the GC-IMS system. Amphetamine, methylone, α-PVP, ketamine, lidocaine, MPHP, cocaine, THJ-2201, and 5F-ADB were employed as model compounds, providing limits of detection from 6 to 15 µg L-1 and recoveries from 70 to 115% for field oral fluids spiked with target analytes at 250, 500, and 600 µg L-1. Moreover, two oral fluid certified reference materials were analysed by the proposed GC-IMS based methodology with obtained relative percentage errors lower than 8.4%, being the proposed GC-IMS procedure a reliable, selective, and sensitive technique for the determination of psychoactive substances in oral fluids.


Subject(s)
Cocaine , Pharmaceutical Preparations , Amphetamine , Cocaine/analysis , Gas Chromatography-Mass Spectrometry , Ion Mobility Spectrometry
9.
Article in English | MEDLINE | ID: mdl-34299908

ABSTRACT

Agricultural activities are highly related to the reduction of the availability of water resources due to the consumption of freshwater for crop irrigation, the use of fertilizers and pesticides. In this study, the water quality of the Adolfo López Mateos (ALM) reservoir was evaluated. This is one of the most important reservoirs in Mexico since the water stored is used mainly for crop irrigation in the most productive agricultural region. A comprehensive evaluation of water quality was carried out by analyzing the behavior of 23 parameters at four sampling points in the period of 2012-2019. The analysis of the spatial behavior of the water quality parameters was studied by spatial distribution graphs using the Inverse Distance Weighting interpolation. Pearson correlation was performed to better describe the behavior of all water quality parameters. This analysis revealed that many of these parameters were significantly correlated. The Principal Components Analysis (PCA) was carried out and showed the importance of water quality parameters. Ten principal components were obtained, which explained almost 90% of the total variation of the data. Additionally, the comprehensive pollution index showed a slight water quality variation in the ALM reservoir. This study also demonstrated that the main source of contamination in this reservoir occurs near sampling point one. Finally, the results obtained indicated that a contamination risk in the waterbody and further severe ecosystem degradations may occur if appropriate management is not taken.


Subject(s)
Water Pollutants, Chemical , Water Quality , Ecosystem , Environmental Monitoring , Mexico , Seasons , Water Pollutants, Chemical/analysis
10.
Anal Chim Acta ; 1167: 338604, 2021 Jul 04.
Article in English | MEDLINE | ID: mdl-34049628

ABSTRACT

In this study, a dual mixed-mode polymer sorbent was prepared via one-step thermally initiated polymerization of 4-vinylpyridine (VP), methacrylic acid (MAA) and ethylene glycol dimethacrylate (EGDMA) for the solid-phase extraction (SPE) of basic and acidic drugs. The use of VP and MAA as ionizable functional monomers allowed the tailoring of ion-exchange and hydrophobic features of the polymer. The obtained polymer was characterized by Fourier-transform infrared spectroscopy and scanning electron microscopy. Next, the retention behavior of dual mixed-mode polymer towards basic and acidic drugs was investigated. Moreover, the practical capability of this novel material was tested for the extraction of relevant drugs such as cocaine, 3-methylmethcathinone, and diazepam in oral fluid samples. Recovery values (at different spiked levels in blank oral fluid samples), ranging from 69 to 99%, and limits of detection (LODs), between 0.10 and 0.25 µg L-1, were obtained.


Subject(s)
Methacrylates , Pharmaceutical Preparations , Polymers , Solid Phase Extraction
11.
J Cosmet Sci ; 72(4): 379-398, 2021.
Article in English | MEDLINE | ID: mdl-35262480

ABSTRACT

Negative health effects of active and passive smokers have been widely described, but the effect of tobacco smoke on the skin has been less explored. In this study, an analytical methodology has been developed to evaluate the dermal permeation of hazardous compounds present in tobacco smoke, using an exposition chamber to simulate finite and infinite smoking conditions, in vitro vertical Franz diffusion cells, and Strat-M® membranes as human skin simulants. Moreover, the antipollution effect of three cosmetics has been evaluated, showing a significant efficacy to reduce dermal permeation of hazardous tobacco-smoke compounds such as of nicotine and aromatic hydrocarbons.


Subject(s)
Cosmetics , Tobacco Smoke Pollution , Skin/chemistry , Smoke/adverse effects , Nicotiana , Tobacco Smoke Pollution/adverse effects , Tobacco Smoke Pollution/analysis
12.
J Cosmet Sci ; 72(1): 33-45, 2021.
Article in English | MEDLINE | ID: mdl-35349424

ABSTRACT

Different a n tipollution products have recently irrupted the market to answer current health concerns related to air contamination. Thus, the development of methodologies for the appropriate evaluation of the efficacy of these products is needed. In this study, an appropriate analytical methodology has been developed and validated for the evaluation of the effectiveness of antipollution cosmetic products against the dermal absorption of different hazardous air pollutants (HAPs). In vitro vertical Franz diffusion cells and Strat-M® as human skin simulants have been used to assess the effectivity of antipollution cosmetic products. An exposition chamber, with a fixed and constant concentration of HAPs, including benzene, toluene, ethylbenzene, and xylene isomers, chlorobenzene, nitrobenzene, haloalkanes, and polycyclic aromatic hydrocarbons, has been designed and made to simulate contaminated atmospheres. The efficacy of antipollution cosmetic products has been evaluated using a multi-pollutant approach, representing a more stringent situation. Diffusion parameters, including flux and lag time, have been calculated for HAPs in the presence of cosmetic samples, using 2 mg product per cm2, and in control tests. The behavior of HAPs followed Fick's first law, allowing the calculation of diffusion parameters. Antipollution effectiveness is demonstrated by statistical evaluation of the diffusion parameters obtained for controls and cosmetics samples. So, a reduction in flux values and an increase in lag times imply an appropriate antipollution effectiveness.


Subject(s)
Air Pollutants , Cosmetics , Air Pollutants/analysis , Humans , Skin/chemistry
13.
J Anal Toxicol ; 45(4): 331-336, 2021 Apr 12.
Article in English | MEDLINE | ID: mdl-32685974

ABSTRACT

A procedure has been developed for the determination of third-generation synthetic cannabinoids in oral fluid samples by using a semi-automated microextraction by packed sorbent (MEPS) procedure and gas chromatography-mass spectrometry (GC-MS) determination. Five synthetic cannabinoids were employed as model compounds 5F-ADB, MMB-CHMICA, THJ-2201, CUMYL-4CN-BINACA and MDMB-CHMCZCA. The most adequate operative conditions for MEPS were evaluated giving quantitative recoveries, from 89 to 124%, in synthetic and field saliva samples spiked with 125 and 250 µg/L of the studied cannabinoids, with the exception of MDMB-CHMCZCA in field saliva samples that provided slightly lower recoveries from 62 to 66%. A high sensitivity was obtained for the proposed MEPS-GC-MS procedure with limits of detection from 10 to 20 µg/L. The obtained results demonstrate the high potential of MEPS-GC-MS combination for semi-automated, selective and sensitive determination of synthetic cannabinoids in oral fluid samples.


Subject(s)
Cannabinoids , Illicit Drugs , Cannabinoids/analysis , Gas Chromatography-Mass Spectrometry , Saliva/chemistry
14.
J Chromatogr A ; 1633: 461615, 2020 Dec 06.
Article in English | MEDLINE | ID: mdl-33099196

ABSTRACT

This review focuses on the existing analytical procedures for the determination of new psychoactive substances (NPS) in biological fluids by chromatographic methods. Direct analysis of samples is scarcely employed and most proposed methodologies include a sample pre-treatment in order to remove matrix interferents and, in some cases, pre-concentrate extracts. Current extraction methods for NPS determination in plasma/serum, urine, and oral fluids have been widely discussed, such as liquid-liquid, solid-phase, and micro extraction approaches, highlighting the advantages and drawbacks of the proposed extraction methodologies. Regarding microextraction approaches, techniques like microextraction by packed sorbent, solid-phase microextraction, miniaturized solid phase extraction, and dispersive liquid-liquid extraction have been proposed for NPS determination in biological fluids with reliable analytical results.


Subject(s)
Body Fluids/chemistry , Clinical Chemistry Tests/methods , Psychotropic Drugs/analysis , Chromatography , Clinical Chemistry Tests/standards , Clinical Chemistry Tests/trends , Humans , Liquid Phase Microextraction , Liquid-Liquid Extraction , Psychotropic Drugs/blood , Psychotropic Drugs/urine , Saliva/chemistry , Solid Phase Extraction , Solid Phase Microextraction , Specimen Handling/standards
15.
J Chromatogr A ; 1610: 460573, 2020 Jan 11.
Article in English | MEDLINE | ID: mdl-31591038

ABSTRACT

A direct procedure based on thermal desorption-gas chromatography-tandem mass spectrometry (TD-GC-MS-MS) was developed for the fast extraction of seven polychlorinated biphenyls (PCBs) from sediments and soils. PCBs were directly extracted, from 20 to 75 mg of sample, without any chemical pre-treatment or use of organic solvents, after the addition of 10 µL internal standard (PCB 195) in acetone. Sample treatment was totally automated. PCBs were extracted at 250 °C for 20 min, using a helium flow and the PCBs were trapped in a cryogenic Tenax trap at -10 °C. After that, analytes were directly desorbed at 270 °C and introduced to the GC-MS-MS system. Recoveries were established using spiked soil and sediment from 2.5 to 50 ng g-1, obtaining values from 74 to 127%. The limits of quantification were from 1.0 to 1.7 ng g-1 for soil and from 0.3 to 0.4 ng g-1 for sediments, respectively. Precision, assessed as the relative standard deviation (RSD), was lower than 8 and 11% for sediment and soil analysis, respectively, except for PCB-28 in soil samples which provided a RSD of 18%. Certified reference material and field samples were analysed by the proposed TD-GC-MS-MS method. Results were compared by a paired samples Student's t-test with those obtained by a reference extraction procedure based on pressurized solvent extraction, followed by stir bar sorptive extraction, being statistically comparable (α = 0.05). A comprehensive greenmetric evaluation of the proposed method was carried out, having the TD extraction a negligible environmental impact as compared to conventional extraction procedures.


Subject(s)
Gas Chromatography-Mass Spectrometry/methods , Geologic Sediments/chemistry , Polychlorinated Biphenyls/analysis , Soil/chemistry , Tandem Mass Spectrometry/methods , Temperature , Humans , Reference Standards , Reproducibility of Results , Soil Pollutants/analysis , Solvents/chemistry
16.
Forensic Sci Int ; 306: 110043, 2020 Jan.
Article in English | MEDLINE | ID: mdl-31743834

ABSTRACT

3',4'-methylenedioxy-2,2-dibromobutyrophenone has been identified and fully characterized in a sample obtained from an anonymous consumer acquired as ketamine through the Internet market. The substance has been deeply characterized by using standard and high performance analytical techniques such as: attenuated total reflectance-infrared spectroscopy, gas chromatography-mass spectrometry, high-resolution mass spectrometry, elemental analysis, and nuclear magnetic resonance, including 1H, 13C, distortionless enhancement by polarization transfer, two dimensional homonuclear 1H-1H correlation spectroscopy, and 1H-13C heteronuclear single-quantum correlation spectra. 3',4'-methylenedioxy-2,2-dibromobutyrophenone is a precursor or intermediate in the synthesis of several synthetic cathinone derivatives, such as pentylone and methylenedioxy pyrovalerone. It is expected that 3',4'-methylenedioxy-2,2-dibromobutyrophenone does not act as psychoactive substance through disruption nor dysregulation of central and peripheral nervous systems, due to the absence of the characteristic amine group of cathinone derivatives. Although it cannot be considered a trend in new psychoactive substances consumption, the presence in the market and the unknown toxicity of this substance makes it a relevant fact.


Subject(s)
Alkaloids/chemistry , Butyrophenones/chemistry , Counterfeit Drugs , Designer Drugs/chemistry , Psychotropic Drugs/chemistry , Chromatography, Liquid , Gas Chromatography-Mass Spectrometry , Humans , Illicit Drugs/chemistry , Internet , Ketamine , Magnetic Resonance Spectroscopy , Spectroscopy, Fourier Transform Infrared
17.
J Chromatogr A ; 1603: 61-66, 2019 Oct 11.
Article in English | MEDLINE | ID: mdl-31262514

ABSTRACT

A simple procedure based on microextraction by packed sorbent (MEPS) has been proposed for the extraction of dichloropane in oral fluids and its determination by ion mobility spectrometry (IMS). Extraction conditions such as type of sorbent (octyl and octadecyl silica), sample pH, number of sample loadings, and elution volume were evaluated to obtain the most appropriate values. Dichloropane was extracted from saliva samples using C8 MEPS, loading with 100 µL sample (adjusted to pH 7) in 4 cycles, washing with 100 µL deionized water, and eluting with 50 µL 2-propanol in 10 cycles. The proposed MEPS procedure has been validated in terms of linearity, accuracy, and precision. A limit of detection of 30 µg L-1 was obtained for dichloropane determination in saliva. The analysis of field and synthetic saliva samples spiked with dichloropane at concentration levels from 250 to 750 µg L-1 provided relative recoveries between 85 and 110%, using the proposed MEPS-IMS procedure. Field oral fluid samples were collected from healthy individuals, blind-spiked from 92 to 278 µg L-1, and analysed by IMS and gas chromatography-mass spectrometry, being the results obtained from both methods statistically comparable. Thus, the proposed MEPS-IMS procedure involves a simple, sensitive, and accurate analysis of dichloropane in saliva.


Subject(s)
Cocaine/analogs & derivatives , Gas Chromatography-Mass Spectrometry/methods , Ion Mobility Spectrometry/methods , Saliva/chemistry , Solid Phase Microextraction/methods , Cocaine/analysis , Humans , Limit of Detection
18.
Anal Chim Acta ; 1052: 73-83, 2019 Apr 04.
Article in English | MEDLINE | ID: mdl-30685044

ABSTRACT

A methamphetamine-based molecularly imprinted polymer (MIP) has been prepared by bulk polymerization to recognize new psychoactive substances (NPS) of the amphetamine, cathinones and 2C families in oral fluid samples, being the first precedent of a synthetized MIP for the extraction and preconcentration 32 NPS including amphetamine type substances and synthetic cathinones from oral fluids. Pre-polymerization complex and resulting materials were appropriately characterized by infrared spectroscopy, scanning electron microscopy, and nitrogen adsorption-desorption isotherms. Appropriateness of the material for the specific recognition of the target analytes was also evaluated through computational calculations and experimentally assessed by solid phase extraction (SPE). The most appropriate SPE conditions were evaluated and recoveries of 32 different NPS were obtained, ranging from 80 to 120% with a relative standard deviation (RSD) in all cases lower than 12%. Amphetamine-related NPS were analyzed by a fast and portable methodology based on ion mobility spectrometry (IMS) and a rearguard procedure based on ultra-high performance liquid chromatography coupled to mass spectrometry (UHPLC-MS) providing limit of detection values from 10 to 80 µg L-1 and from 0.03 to 1.3 µg L-1, respectively. Oral fluid samples, containing different interferents like caffeine, fluticasone and cetirizine, were spiked with 300 µg L-1 amphetamine and subsequently analyzed, showing recoveries ranging from 81 to 115% using both methodologies. Thus, this paper shows preliminary results to demonstrate the applicability of the developed procedure which could be used with minor modifications as screening technique in on-road drug analysis.


Subject(s)
Amphetamine/analysis , Amphetamine/isolation & purification , Body Fluids/chemistry , Chemical Fractionation/methods , Molecular Imprinting , Solid Phase Extraction/methods , Adsorption , Amphetamine/chemistry , Central Nervous System Stimulants/analysis , Central Nervous System Stimulants/chemistry , Central Nervous System Stimulants/isolation & purification , Green Chemistry Technology , Humans , Polymerization
19.
Talanta ; 190: 321-326, 2018 Dec 01.
Article in English | MEDLINE | ID: mdl-30172516

ABSTRACT

A simple, quick and low cost procedure was developed for the extraction of Δ9-tetrahydrocannabinol, cannabidiol, and cannabinol from marijuana samples, based on the use of a hard-cap espresso extraction with 2-propanol. After extraction, cannabinoids were directly determined after appropriate dilution by gas-chromatography-mass spectrometry, reaching a limit of detection from 0.03 to 0.05 mg g-1. Extraction efficiency was evaluated by the comparison of results obtained for seized samples by the proposed method and a reference methodology based on ultrasound-assisted extraction. Moreover, ion mobility was proposed for the rapid and sensitive determination of Δ9-tetrahydrocannabinol and cannabidiol providing a quick response for the analysis of seized marijuana samples in 1 min, including extraction, dilution and determination.


Subject(s)
Cannabinoids/isolation & purification , Cannabis/chemistry , Chemical Fractionation/instrumentation , Cannabinoids/chemistry , Coffee/chemistry , Gas Chromatography-Mass Spectrometry , Humans , Time Factors
20.
Anal Bioanal Chem ; 410(23): 5961-5967, 2018 Sep.
Article in English | MEDLINE | ID: mdl-29982933

ABSTRACT

The advantages of using smart materials as immunosorbents in the analysis of complex matrices by ion mobility spectrometry (IMS) have been highlighted in this study. A novel analytical method has been proposed for the sensitive, selective, and fast determination of residues of the plant growth regulator forchlorfenuron in fruit juices. Three different monoclonal antibodies (s3#22, p2#21, and p6#41) were employed for the production of immunosorbents, based on Sepharose gel beads, which were characterized in terms of loading capacity, solvent resistance, and repeatability for its use in solid-phase extraction (SPE). Immunosorbents that were prepared with antibody p6#44 provided the best performance, with a loading capacity of 0.97 µg, a 10% (v/v) 2-propanol tolerance, and a reusability of at least eight uses. The SPE procedure involved the use of a column with 0.15 g Sepharose beads, containing 0.5 mg antibody, which was loaded to 20 mL of the sample, washed with 2 mL of water plus 2 mL of 10% (v/v) 2-propanol, and eluted with 2 mL of 2-propanol. The cleaned extract was directly analyzed by IMS, giving a limit of detection of 2 µg L-1 with a relative standard deviation of 7.6%. Trueness was assessed by the analysis of blank grape and kiwifruit juice samples spiked with forchlorfenuron concentrations from 10 to 400 µg L-1, with recoveries from 80 to 115%. The analytical performance of the proposed immunosorbent was compared with conventional extraction and cleanup methods, such as QuEChERS and C18-based SPE, giving the cleanest extracts for accurate determinations of forchlorfenuron by IMS. Graphical abstract ᅟ.


Subject(s)
Food Analysis/methods , Fruit and Vegetable Juices/analysis , Immunosorbents/chemistry , Ion Mobility Spectrometry/methods , Phenylurea Compounds/analysis , Plant Growth Regulators/analysis , Pyridines/analysis , Solid Phase Extraction/methods , Antibodies, Monoclonal/chemistry , Equipment Design , Limit of Detection , Solid Phase Extraction/instrumentation
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