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1.
Bull Environ Contam Toxicol ; 112(5): 74, 2024 May 11.
Artigo em Inglês | MEDLINE | ID: mdl-38733375

RESUMO

Polycyclic aromatic hydrocarbons (PAHs), dust, and wax were measured in pine needles, and PAHs were also measured in surface soil. Pearson correlation analysis was performed between the analytical values. The main compounds responsible for the increase in total PAHs were non-carcinogenic phenanthrene and fluoranthene. Therefore, the % content of carcinogenic PAHs decreased with a slope = -0.037 (r = 0.47, p < 0.01), as the total PAH concentration in pine needles increased. Correlations between individual PAHs in pine needles and surface soil were very high when only low-number ring PAHs (2R- and 3R-PAHs) were statistically analyzed and significant when only high-number ring PAHs were statistically analyzed. Low-number ring PAH mainly moves in the gas phase and diffuses into the wax layer, so it was found to be statistically significant with the wax content of pine needles. High-number ring PAHs showed a high correlation with the amount of dust in pine needles because they mainly attached to dust particles and accumulated on the surface of pine needles. The ratios of fluoranthene/pyrene and methylphenanthrene/phenanthrene for predicting the origin of atmospheric PAHs have also been proven valid for pine needles.


Assuntos
Monitoramento Ambiental , Pinus , Hidrocarbonetos Policíclicos Aromáticos , Hidrocarbonetos Policíclicos Aromáticos/análise , Pinus/química , República da Coreia , Folhas de Planta/química , Fenantrenos/análise , Poluentes do Solo/análise , Poluentes Atmosféricos/análise
2.
Anal Bioanal Chem ; 416(6): 1363-1374, 2024 Mar.
Artigo em Inglês | MEDLINE | ID: mdl-38285226

RESUMO

Several countries have exempted synthetic nicotine from existing regulatory frameworks, resulting in the widespread substitution of synthetic nicotine (SN) in almost all e-cigarette products available. However, it remains uncertain whether the purported synthetic nicotine is indeed genuine SN. There is a need to develop biological indicators and an analytical method that more clearly distinguishes between the two sources. Impurities in neat tobacco-derived nicotine (TDN) were characterized and identified through non-targeted and targeted analysis. Gas chromatography-tandem mass spectrometry (GC-MS/MS) conditions were optimized for detecting biological indicators in e-cigarette products. Nine tobacco-related alkaloids were identified and selected as biological indicators for TDN. A liquid-liquid extraction and GC-MS/MS quantitative method were developed to detect nine biological indicators in e-cigarette products with the limit of quantification ranging from 0.2 to 4.2 µg L-1 using 0.5 mL of e-liquid. This method was applied to 50 e-cigarette brands purchased in the Korean market. The developed method was able to easily and accurately identify the origin of nicotine even using a small amount of e-liquid sample. It is expected that effective e-cigarette regulation will be possible if the nicotine biological indicator and high-sensitivity analysis method developed in this study are used.


Assuntos
Sistemas Eletrônicos de Liberação de Nicotina , Nicotina , Nicotina/análise , Biomarcadores Ambientais , Espectrometria de Massas em Tandem/métodos , Cromatografia Gasosa-Espectrometria de Massas
3.
J Korean Med Sci ; 38(45): e391, 2023 Nov 20.
Artigo em Inglês | MEDLINE | ID: mdl-37987110

RESUMO

BACKGROUND: Phthalates and bisphenol A (BPA) are endocrine-disrupting chemicals and may cause immunological disorders in children. Therefore, according to the region, we investigated urinary phthalates and BPA levels and the relationship between urinary phthalate, aeroallergen sensitization, and eosinophil count during the coronavirus disease 2019 pandemic. METHODS: In total, 203 schoolchildren (134 residential and 69 industrial) aged 7-10 years were enrolled between July 2021 and July 2022. The BPA, metabolites of four high-molecular-weight phthalates (Σ4HMWP) and three low-molecular-weight phthalates (Σ3LMWP), were measured in the urine samples. Total eosinophil count and transepidermal water loss (TEWL) were also measured along with the skin prick test. RESULTS: The two groups had no differences in terms of BPA. The industrial group had significantly more plastic container usage, and there was a difference in the Σ3LMWP (P < 0.001) between the two groups but no difference in the Σ4HMWP (P = 0.234). The quartiles of urinary Σ4HMWP and Σ3LMWP (P < were not associated with the total eosinophil count, vitamin D level, or TEWL. After adjusting for cofactors, the quartiles of urinary Σ4HMWP and Σ3LMWP were significantly associated with total eosinophil count (P < 0.001) but not with aeroallergen sensitization or vitamin D. CONCLUSION: Exposure to phthalates was significantly associated with eosinophil count but not with aeroallergen sensitization or vitamin D. Therefore, reducing the use of plastic containers may effectively prevent exposure to phthalates and reduce Th2 cell-mediated inflammation in children.


Assuntos
Poluentes Ambientais , Ácidos Ftálicos , Criança , Humanos , Eosinófilos/metabolismo , Ácidos Ftálicos/urina , Vitamina D , Compostos Benzidrílicos/urina , Exposição Ambiental/efeitos adversos
4.
Environ Monit Assess ; 194(4): 268, 2022 Mar 09.
Artigo em Inglês | MEDLINE | ID: mdl-35266055

RESUMO

The simultaneous determination of 8 polychlorinated biphenyls (PCBs), 23 organic chlorine pesticides (OCPs), and 35 polycyclic aromatic hydrocarbons (PAHs) in black-tailed gull eggs was described using ultrasound-assisted extraction and gas chromatography-tandem mass spectrometry (GC-MS/MS). The ranges of the lower limits of detection for PCBs, OCPs, and PAHs were 0.006-0.029, 0.01-0.10, and 0.01-0.20 µg kg-1, respectively. The intraday precision was in the range of 0.650-12.9% and the intraday accuracy was in the range of 86.6-113%. When the proposed method was used to analyze the target compounds in gull eggs collected from six sites in the Republic of Korea, the analytical results demonstrated concentration ranges of 113.32-394.07 µg kg-1 for total PCBs, 422.92-1082.09 µg kg-1 for total OCPs, and 134.50-231.27 µg kg-1 for total PAHs in the samples. The PCA results for PAHs and OCPs were well differentiated by sampling site, whereas those for PCBs differed little by sampling site. There were more pyrogenic PAHs in the West Sea and the South Sea with many industrial areas than in the East Sea with few industrial areas. Differences in the OCP patterns of samples from the West Sea close to China were considered to be related to the use of DDT in China until recently. PCBs were accumulated in the samples regardless of region, so there was no significant difference in the PCB patterns between the samples obtained from the three Seas.


Assuntos
Charadriiformes , Hidrocarbonetos Clorados , Praguicidas , Bifenilos Policlorados , Hidrocarbonetos Policíclicos Aromáticos , Animais , Cloro/análise , Monitoramento Ambiental , Cromatografia Gasosa-Espectrometria de Massas , Hidrocarbonetos Clorados/análise , Praguicidas/análise , Bifenilos Policlorados/análise , Hidrocarbonetos Policíclicos Aromáticos/análise , Espectrometria de Massas em Tandem
5.
Biomed Chromatogr ; 36(6): e5360, 2022 Jun.
Artigo em Inglês | MEDLINE | ID: mdl-35261063

RESUMO

A method to determine 8 polychlorinated biphenyls (PCBs), 23 organochlorine pesticides (OCPs) and 16 polycyclic aromatic hydrocarbons (PAHs) was described using dispersive liquid-liquid microextraction (DLLME) of a small amount of plasma or serum sample and gas chromatography-tandem mass spectrometry (GC-MS/MS). The appropriate selection of the extraction solvent and dispersing solvent contributes to a high extraction yield and a clean extract. To verify the developed method, the interference, linearity of the calibration curve, detection limit, precision and accuracy were evaluated. The calibration curves were linear by 2-3 orders of magnitude with correlation coefficients above 0.997 in all cases. The LODs of PCBs, OCPs and PAHs were measured in the ranges of 0.0006-0.0029, 0.001-0.029 and 0.0002-0.012 ng/mL. The intraday precision achieved by this method was 2.19-10.3% (PCBs), 1.65-14.3% (OCPs) and 0.91-12.8% (PAHs), and the intraday accuracy 1.56-7.37% (PCBs), 2.34-19.6% (OCPs) and 1.49-15.7% (PAHs). The advantage of this method is that the analysis of PCBs, OCPs, and PAHs can be performed in a single chromatographic run, and the low detection limit enables monitoring of target substances in low exposure general public samples, and the analysis procedure is relatively simple and fast.


Assuntos
Hidrocarbonetos Clorados , Microextração em Fase Líquida , Praguicidas , Bifenilos Policlorados , Hidrocarbonetos Policíclicos Aromáticos , Cromatografia Gasosa-Espectrometria de Massas/métodos , Humanos , Hidrocarbonetos Clorados/análise , Praguicidas/análise , Hidrocarbonetos Policíclicos Aromáticos/análise , Solventes/análise , Espectrometria de Massas em Tandem
6.
J Mass Spectrom ; 57(2): e4811, 2022 Jan 17.
Artigo em Inglês | MEDLINE | ID: mdl-35088484

RESUMO

Tobacco flavors increase the attractiveness of a tobacco brand and ultimately promote addiction. Information about what flavor and how much flavor is in flavor capsules can provide an effective way to regulate tobacco flavor. In this study, 128 flavor chemicals were identified and quantified by gas chromatography-mass spectrometry using libraries and authentic standards. Validation of the developed method was performed for interference, detection limits, calibration curves, accuracy, and precision. Menthol was the main ingredient in all capsules, and the carcinogenic pulegone was detected. Detected menthofuran, benzyl alcohol, geraniol, and eugenol cause toxic or severe irritation, and detected lactones can increase nicotine addiction by inhibiting nicotine metabolism in smokers. Margin of exposures for carcinogenic pulegone and non-carcinogenic menthol were well below safety thresholds, indicating a significant risk of inhalation exposure. It is desirable to prohibit the use of flavor capsules in consideration of human risk.

7.
J AOAC Int ; 105(1): 62-68, 2022 Feb 04.
Artigo em Inglês | MEDLINE | ID: mdl-34529053

RESUMO

BACKGROUND: Alkylhydrazines are widely used in industrial fields. An analysis of alkylhydrazines in surface water is needed because these chemicals are likely to be discharged into wastewater and enter aquatic environments. OBJECTIVE: An ultra-high performance liquid chromatography (UHPLC)-tandem mass spectrometry (MS/MS) method was developed to determine the levels of five alkylhydrazines (N, N-dimethylhydrazine, ethylhydrazine, 1-isopropylhydrazine, phenylhydrazine, and 1-methyl-1-phenylhydrazine) in surface water. METHODS: This method is based on the derivatization of alkylhydrazines with 1-nitro-2-naphthaldehyde (NNA) in water. A derivatization reagent dosage of 0.5 mg NNA, a pH of 2, and a reaction time of 30 min at 40°C were determined to be the optimal conditions for UHPLC-MS/MS detection. The derivatives were injected into the LC system without additional extraction or purification steps. RESULTS: The proposed method was used under optimized conditions to detect alkylhydrazines in surface water, with the limit of quantification found to be 0.01-0.03 µg/L. The accuracy ranged from 91.0 to 106.0%, and the precision, expressed as the relative standard deviation, was less than 10%. Of the five alkylhydrazines, only N, N-dimethyl hydrazine was detected in the real samples at a concentration range of 0.010-0.041 µg/L. CONCLUSION: The developed method can be used to confirm the presence of alkylhydrazine residues in surface water and represents an important tool for evaluating the fate of alkylhydrazines in surface water. HIGHLIGHTS: A UHPLC-MSMS method was developed in order to dtermine the alkylhydrazine in surface water after derivatization without an extraction or cleanup step.


Assuntos
Espectrometria de Massas em Tandem , Água , Aldeídos , Cromatografia Líquida de Alta Pressão , Naftalenos , Extração em Fase Sólida
8.
J Pharm Biomed Anal ; 207: 114397, 2022 Jan 05.
Artigo em Inglês | MEDLINE | ID: mdl-34626940

RESUMO

A gas chromatography-mass spectrometric (GC-MS) method was developed for the qualitative and quantitative analysis of flavor chemicals in tobacco heating products (THPs), traditional tobacco products (TTPs) and their flavoring capsules. A total of 283 compounds were identified through non-target analysis, and the final 302 compounds were selected to develop an analytical method. The lower limits of detection (LOD) of analytes were 0.00074-12 mg/kg and their LOD range was wide depending on the presence or absence in the reference cigarette. The precision of the 302 compounds was less than 24.5%, and the accuracy ranged from 80.0% to 120%. A total of 190 flavors and 5 contaminants were determined in 21 THP, 10 TTP, 8 THP capsules and 11 TTP capsules. When comparing the total flavor content of flavors per cigarette, it was in the order of THP capsule> TTP capsule ≫ THP ≫ TTP. The correlations between the 53 cigarette products and 190 flavor chemicals were analyzed using PCA. It has been demonstrated that PCA results can be a useful tool in differentiating brands and manufacturers of tobacco products.


Assuntos
Sistemas Eletrônicos de Liberação de Nicotina , Produtos do Tabaco , Cápsulas , Aromatizantes , Calefação , Nicotiana
9.
Artigo em Inglês | MEDLINE | ID: mdl-32811350

RESUMO

A method for the simultaneous determination in mussel of 8 polychlorinated biphenyls (PCBs), 23 organochlorine pesticides (OCPs), and 35 polycyclic aromatic hydrocarbons (PAHs), including alkyl-PAHs, was optimised using ultrasound-assisted cloudy extraction and gas chromatography-tandem mass spectrometry (GC-MS/MS). Optimal selection of the extraction solvent and the dispersing solvent contributed to a high extraction yield and a clean extract. The ranges of the lower limits of detection of PCBs, OCPs and PAHs were 0.012-0.058, 0.01-0.29 and 0.01-0.5 µg kg-1, respectively. The feasibility of the proposed method was validated by analysing standard reference materials of mussel with satisfactory results. The precision achieved by this method was in the range of 0.677-2.69% (PCBs), 1.14-6.60% (OCPs) and 0.694-7.46% (PAHs), and its accuracy was in the range of 101-104% (PCBs), 99.6-106% (OCPs) and 101-110% (PAHs). The advantages of the method include the simultaneous measurement of 66 analytes and the simplicity, low cost and high sensitivity of the procedure. When the proposed method was used to analyse the target compounds in 11 mussel samples, the analytical results displayed a concentration range of 0.41-0.45 µg kg-1 for PCBs, 0.26-6.49 µg kg-1 for OCPs, and 3.48-30.69 µg kg-1 for PAHs.


Assuntos
Bivalves/química , Hidrocarbonetos Clorados/análise , Praguicidas/análise , Bifenilos Policlorados/análise , Hidrocarbonetos Policíclicos Aromáticos/análise , Animais , Cromatografia Gasosa , Espectrometria de Massas em Tandem , Ondas Ultrassônicas
10.
J Pharm Biomed Anal ; 189: 113460, 2020 Sep 10.
Artigo em Inglês | MEDLINE | ID: mdl-32663759

RESUMO

N-Nitrosodimethylamine (NDMA) has been detected in some drug substance and drug products containing sartans, ranitidine and metformin. N-nitrosodiethylamine (NDEA) has also been found to be present in some sartan medications. A method for the simultaneous detection of NDMA and NDEA in drug substances and finished products of sartans, metformin and ranitidine has been optimized using isotope dilution, clean-up procedure and gas chromatography-tandem mass spectrometry (GC-MS/MS). The purification of drug substances and excipients was efficient when utilizing precipitation and activated charcoal cartridges. Most of irbesartan, pimasartan, olmesartan, and candesartan were removed by precipitation using solubility difference, while valsartan, rosartan, metformin and ranitidine were completely removed after activated charcoal purification. Even when the extracts were injected in GC-MS/MS more than 100 times, the peak shape and sensitivity did not change, and no peak interference occurred. When a 0.10 g sample was used, the range of the lower limit of detection was 0.07-0.3 µg/kg, and the range of the lower limit of quantification was 0.3-0.9 µg/kg. The precision was in the range of 0.4-2.7 % for NDMA and 0.4-4.2 % for NDEA, and the accuracy was in the range of 95.0-105 % for NDMA and 93.6-104 % for NDEA. NDMA was detected with a concentration of 0.004 mg/kg in a valsartan and 0.012 mg/kg in a ranitidine, and NDEA was detected at concentrations of 0.009 and 0.008 mg/kg in irbesartan and rosartan. Otherwise, NDMA was detected at a concentration of 0.062 mg/kg in a fimasartan product and 0.009 mg/kg in a ranitidine product. This method is available for all drug substances and finished products of sartans; metformin and ranitidine.


Assuntos
Metformina , Preparações Farmacêuticas , Bloqueadores do Receptor Tipo 1 de Angiotensina II , Dimetilnitrosamina/análogos & derivados , Dimetilnitrosamina/análise , Cromatografia Gasosa-Espectrometria de Massas , Ranitidina , Extração em Fase Sólida , Espectrometria de Massas em Tandem
11.
J Expo Sci Environ Epidemiol ; 30(5): 888-897, 2020 09.
Artigo em Inglês | MEDLINE | ID: mdl-31300710

RESUMO

Mold stain remover (MSR) is used to clean mold and mildew spots from surfaces and contains a variety of chemical substances. In this study, we estimated the inhalation and dermal exposures associated with the use of trigger spray MSRs, and performed screening-level risk assessments for the use of this type of product in Korea. Inhalation and dermal exposures were estimated using exposure algorithms based on exposure factors obtained from a nationwide survey of 10,000 participants and chemical analyses of the four most popular trigger spray MSRs. The hazard quotients (HQs) for noncancer risk and excess cancer risk (ECR) were calculated for each chemical. The mean inhalation exposure estimates for formaldehyde, benzene, chloroform, and carbon tetrachloride were 6.9 × 10-7, 1.7 × 10-7, 5.4 × 10-6, and 2.7 × 10-5 mg/kg/day, respectively. Dermal exposures of the chemicals were 5.7-6.5 times higher than inhalation exposures. The HQs for total exposure were all below 1, which indicated little noncancer risk from the use of MSRs. The safe ECR value of 1 × 10-6, was exceed in one subject for inhalation exposure of benzene and four subjects for dermal exposure of formaldehyde, while 19.8% for dermal exposure of benzene were above this value. Therefore, use of trigger spray MSRs in Korea should require more detailed exposure and risk assessment, especially for benzene.


Assuntos
Benzeno , Exposição por Inalação , Humanos , Exposição por Inalação/efeitos adversos , Exposição por Inalação/análise , República da Coreia , Medição de Risco
12.
J Pharm Biomed Anal ; 174: 115-122, 2019 Sep 10.
Artigo em Inglês | MEDLINE | ID: mdl-31163345

RESUMO

Benzene (B), toluene (T), ethylbenzene (E), o-, m- and p-xylene (o-, m-, p-X) are ubiquitous and frequently exposed to human throughout the environment. Previously published test methods for phenolic biomarkers are not sensitive enough to be detected in most general population groups and require a lot of labor. A simple and convenient headspace solid-phase microextraction (HS-SPME) gas chromatography-mass spectrometry method was described for the simultaneous determination of 15 hydroxyl biomarkers of BTEX in urine. Hydroxyl biomarkers in urine were vaporized and adsorbed onto a selected fiber after enzyme hydrolysis with ß-glucuronidase/arylsulfatase. The optimal HS-SPME conditions were achieved with an 85-µm-carboxen-polydimethylsiloxane fiber, an extraction temperature of 70 °C, a heating time of 30 min, and a pH of 4.0. The desorption was performed for 1 min at 250 °C. Under the established conditions, the lowest limits of detection were from 0.02 to 0.15 µg/L in 5.0 mL of urine, and the intra- and inter-day relative standard deviations were less than 12.7% at 0.5, 2.0, 50, and 200 µg/L. The calibration curve demonstrated good linearity with greater than r2 = 0.99 in synthetic urine. This method is convenient, simple, environmentally friendly, and amenable to automation.


Assuntos
Derivados de Benzeno/urina , Benzeno/química , Biomarcadores/urina , Tolueno/urina , Xilenos/urina , Adolescente , Calibragem , Criança , Pré-Escolar , Cromatografia Gasosa-Espectrometria de Massas , Humanos , Concentração de Íons de Hidrogênio , Íons , Limite de Detecção , Modelos Lineares , Reprodutibilidade dos Testes , Microextração em Fase Sólida , Temperatura , Urinálise
13.
J Sep Sci ; 40(20): 3958-3968, 2017 Oct.
Artigo em Inglês | MEDLINE | ID: mdl-28834364

RESUMO

Malondialdehyde has been used as a biomarker for lipid peroxidation in biological samples. An ultra-high performance liquid chromatography with tandem mass spectrometry method was developed to determine the levels of malondialdehyde in human urine and saliva samples. To select the optimum derivatization reagent from four diamino compounds, the reactivity and sensitivity of their derivatives were compared, and 3,4-diaminobenzophenone was selected. The optimum reaction conditions for malondialdehyde with 3,4-diaminobenzophenone were as follows: a reagent dosage of 50 mg/L, pH of 4, and reaction for 30 min at 50°C. The formed derivative product was analyzed using ultra-high performance liquid chromatography with tandem mass spectrometry without additional extraction or concentration steps. In the optimal conditions, the method was used to determine malondialdehyde concentration in human urine and saliva samples. The limits of quantification for malondialdehyde in biological samples were over a concentration range of 0.1-0.3 µg/L. Additionally, the calibration curve showed a linearity greater than r2  = 0.997. The method was used to analyze 14 human urine and saliva samples from healthy volunteers. Malondialdehyde was detected in the concentration range of 1.7-33.6 µg/g creatinine in all human urine samples and 0.1-1.3 µg/L in all human saliva samples.


Assuntos
Malondialdeído/análise , Malondialdeído/urina , Saliva/química , Benzofenonas , Cromatografia Líquida de Alta Pressão , Humanos , Fenilenodiaminas , Espectrometria de Massas em Tandem
14.
Chemosphere ; 174: 157-164, 2017 May.
Artigo em Inglês | MEDLINE | ID: mdl-28161516

RESUMO

Seven halogenated volatile organic compounds (HVOCs) and two haloacetic acids were detected and quantified in 15 household products, including sodium hypochlorite, by gas chromatography-mass spectrometry (GC-MS). Chloroform was detected in a range of 0.2-30.2 mg kg-1 in all products, and carbon tetrachloride was observed in 13 samples in a range of 0.05-352 mg kg-1. Dichloroacetic acid and trichloroacetic acid were also detected up to 94 and 146 mg kg-1 in household products. The estimated human exposures of chloroform, carbon tetrachloride, dichloroacetic acid and trichloroacetic acid were calculated to 0.041, 0.240, 0.913 and 2.39 mg/kg/day by the exposure algorithm from the Japan National Institute of Technology and Evaluation, respectively. According to the calculated result, the total estimated human exposure of chloroform were determined to exceed the tolerable concentration of inhalation exposure presented by the World Health Organization. The DBPs should be controlled to the lowest concentrations in the chlorine-containing household cleansing products.


Assuntos
Cloro/química , Desinfetantes/análise , Desinfetantes/química , Produtos Domésticos/análise , Compostos Orgânicos Voláteis/análise , Desinfecção/métodos , Cromatografia Gasosa-Espectrometria de Massas , Humanos , Japão , Compostos Orgânicos Voláteis/química
15.
J Chromatogr Sci ; 55(2): 109-116, 2017 02.
Artigo em Inglês | MEDLINE | ID: mdl-27799251

RESUMO

As the popularity of body art including tattoo ink has increased, the safety associated with it has become an important interest. In this study, twenty volatile organic compounds (VOCs) and two aldehydes in tattoo inks were identified and quantified. Headspace and gas chromatography-mass spectrometry (HS GC-MS) for the VOCs and HS GC-MS based on derivatization with 2,2,2-trifluoroethylhydrazine (TFEH) for aldehydes was developed. Benzene, chloroform, toluene, ethylbenzene, m-xylene, p-xylene, o-xylene, propylbenzene, chlorobenzene, tert-butylbenzene, 1,3,5-trimethylbenzene, styrene, 1,2,4-trimethylbenzene, 2-chlorotoluene, 4-chlorotoluene, 1,3-dichlorobenzene, 1,4-dichlorobenzene, 1,2-dichlorobenzene, 1,2,4-trichlorobenzene and isopropyl alcohol were detected with the concentration range of 0.02-207,000 mg/kg in 16 different tattoo inks. Formaldehyde and acetaldehyde were detected with the concentration range of 0.4-308 mg/kg in the same samples. Our analytical results represent solvents used intentionally or non-intentionally in tattoo inks, and thus they may provide important information for national regulation.


Assuntos
Aldeídos/análise , Tinta , Tatuagem , Compostos Orgânicos Voláteis/análise , Cromatografia Gasosa-Espectrometria de Massas/métodos , Limite de Detecção , Modelos Lineares , Reprodutibilidade dos Testes
16.
Anal Chim Acta ; 950: 57-63, 2017 Jan 15.
Artigo em Inglês | MEDLINE | ID: mdl-27916130

RESUMO

A headspace solid-phase micro extraction (HS-SPME) and gas chromatography-tandem mass spectrometric (GC-MS/MS) method is described to detect hydrazine after derivatization with 1,1,1-trifluoro-2,4-pentanedione (1,1,1-TFPD) to 3-methyl-5-(trifluoromethyl) pyrazole in industrial waste water. The following optimal HS-SPME conditions were used: 85 µm-carboxen-polydimethylsiloxane fibre, 100 mg L-1 TFPD, saturated NaCl, an extraction/derivatization temperature of 80 °C, a heating time of 40 min, and a pH of 9.5. Under the established conditions, the detection and quantification limits were 0.002 µg L-1 and 0.007 µg L-1 by using 5 mL of waste water and the intra- and inter-day relative standard deviations were less than 10.2% at concentrations of 0.02 and 0.1 µg L-1. The calibration curve showed good linearity, with r2 = 0.998; the accuracy was in the range of 98.0-103%; and the precision of the assay was less than 10.2% in industrial waste water. Hydrazine was detected over a concentration range of 0.011-0.074 µg L-1 in 5 of 20 waste water samples.

17.
Anal Bioanal Chem ; 409(5): 1247-1256, 2017 Feb.
Artigo em Inglês | MEDLINE | ID: mdl-27826631

RESUMO

An analytical method for the detection of 14 volatile organic compounds (VOCs) was developed to investigate VOCs in refill fluids and cartridges of electronic cigarettes (EC) using headspace solid-phase micro extraction (HS-SPME) coupled with gas chromatography-mass spectrometry (GC-MS). In total, 14 VOCs were identified and quantified in 283 flavored liquids, 21 nicotine liquids, and 12 disposable cartridges. The detected concentration ranges of the VOCs are as follows: benzene (0.008-2.28 mg L-1), toluene (0.006-0.687 mg L-1), ethylbenzene (0.01-1.21 mg L-1), m-xylene (0.002-1.13 mg L-1), p-xylene (0.007-2.8 mg L-1), o-xylene (0.004-2.27 mg L-1), styrene (0.011-0.339 mg L-1), ethyl acetate (0.3-669.9 mg L-1), ethanol (16-38,742 mg L-1), methanol (66-3375 mg L-1), pyridine (0.077-99.7 mg L-1), acetylpyrazine (0.077-147 mg L-1), 2,3,5-trimethylpyrazine (0.008-96.8 mg L-1), and octamethylcyclotetrasiloxane (0.1-57.2 mg L-1). Benzene, toluene, ethylbenzene, m-xylene, p-xylene, and o-xylene coexisted in samples, which may have originated from the use of petrogenic hydrocarbons as an extraction solvent for flavor and nicotine from natural plants. The maximum detected concentrations of benzene, methanol, and ethanol in liquid samples were found in quantities higher than their authorized maximum limits as residual solvents in pharmaceutical products.


Assuntos
Álcoois/análise , Sistemas Eletrônicos de Liberação de Nicotina , Cromatografia Gasosa-Espectrometria de Massas/métodos , Microextração em Fase Sólida/métodos , Compostos Orgânicos Voláteis/análise
18.
J Cancer Prev ; 21(3): 187-193, 2016 Sep.
Artigo em Inglês | MEDLINE | ID: mdl-27722145

RESUMO

BACKGROUND: Despite major advances in lung cancer treatment, early detection remains the most promising way of improving outcomes. To detect lung cancer in earlier stages, many serum biomarkers have been tested. Unfortunately, no single biomarker can reliably detect lung cancer. We combined a set of 2 tumor markers and 4 inflammatory or metabolic markers and tried to validate the diagnostic performance in lung cancer. METHODS: We collected serum samples from 355 lung cancer patients and 590 control subjects and divided them into training and validation datasets. After measuring serum levels of 6 biomarkers (human epididymis secretory protein 4 [HE4], carcinoembryonic antigen [CEA], regulated on activation, normal T cell expressed and secreted [RANTES], apolipoprotein A2 [ApoA2], transthyretin [TTR], and secretory vascular cell adhesion molecule-1 [sVCAM-1]), we tested various sets of biomarkers for their diagnostic performance in lung cancer. RESULTS: In a training dataset, the area under the curve (AUC) values were 0.821 for HE4, 0.753 for CEA, 0.858 for RANTES, 0.867 for ApoA2, 0.830 for TTR, and 0.552 for sVCAM-1. A model using all 6 biomarkers and age yielded an AUC value of 0.986 and sensitivity of 93.2% (cutoff at specificity 94%). Applying this model to the validation dataset showed similar results. The AUC value of the model was 0.988, with sensitivity of 93.33% and specificity of 92.00% at the same cutoff point used in the validation dataset. Analyses by stages and histologic subtypes all yielded similar results. CONCLUSIONS: Combining multiple tumor and systemic inflammatory markers proved to be a valid strategy in the diagnosis of lung cancer.

19.
J Chromatogr A ; 1448: 115-120, 2016 May 27.
Artigo em Inglês | MEDLINE | ID: mdl-27130584

RESUMO

A simple and convenient headspace solid-phase microextraction (HS-SPME) gas chromatography mass spectrometry (GC-MS) method was described for the determination of glutaraldehyde in water. Glutaraldehyde in water reacted with 2,2,2-trifluoroethylhydrazine (TFEH) in a headspace vial and the formed TFEH derivatives were vaporized and adsorbed onto a fiber. The optimal HS-SPME conditions were achieved with a 50/30µm-divinylbenzene-carboxen-polydimethylsiloxane fiber, 0.06% 2,2,2-TFEH, 25% salt, an extraction/derivatization temperature of 80°C, a heating time of 30min, and a pH of 6.5. The desorption was performed for 1min at 240°C. Under the established conditions, the lowest limits of detection were 0.3µg/L and 0.1µg/L in 6.0mL of surface water and drinking water, respectively, and the intra- and inter-day relative standard deviation was less than 9.1% at concentrations of 50, 100 and 500µg/L. The calibration curve showed good linearity with R=0.9995 and R=0.9993 in surface water and drinking water, respectively. This method is simple, amenable to automation and environmentally friendly.


Assuntos
Glutaral/análise , Hidrazinas/química , Poluentes Químicos da Água/análise , Dimetilpolisiloxanos , Cromatografia Gasosa-Espectrometria de Massas/métodos , Indicadores e Reagentes , Polivinil , Microextração em Fase Sólida/métodos , Temperatura
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