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1.
Se Pu ; 42(8): 805-811, 2024 Aug.
Artigo em Chinês | MEDLINE | ID: mdl-39086250

RESUMO

Tobacco flavor, an important tobacco additive, is an essential raw material in cigarette production that can effectively improve the quality of tobacco products, add aroma and taste, and increase the suction flavor. The quality consistency of tobacco flavors affects the quality stability of branded cigarettes. Therefore, the quality control of tobacco flavors is a major concern for cigarette and flavor manufacturers. Physical and chemical indices, odor similarity, and sensory efficacy are employed to evaluate the quality of tobacco flavors, and the analysis of chemical components in tobacco flavors is usually conducted using gas chromatography (GC) and high performance liquid chromatography (HPLC). However, because the composition of tobacco flavors is complex, their quality cannot be fully reflected using a single component or combination of components. Therefore, establishing an objective analytical method for the quality control of tobacco flavors is of extreme importance. Chromatographic fingerprint analysis is routinely used for the discriminative analysis of tobacco flavors. Chromatographic fingerprints refer to the general characteristics of the concentration profiles of different chemical compounds. In the daily procurement process, fingerprints established by GC and HPLC are effective for the evaluation and identification of tobacco flavors. However, given continuous improvements in aroma-imitation technology, some flavors with high similarity cannot be directly distinguished using existing methods. In this study, a method for the determination of organic acids and inorganic anions in tobacco flavors based on ion chromatography (IC) was developed to ensure the quality consistency of tobacco flavors. A 1.0 g sample of tobacco flavors and 10 mL of deionized water were mixed and vibrated for 30 min. The aqueous sample solution was passed through a 0.45 µm membrane filter and RP pretreatment column in succession to eliminate interferences and then subjected to IC. Standard solutions containing nine organic acids and seven inorganic anions were used to identify the anions in the tobacco flavors, and satisfactory reproducibility was obtained. The relative standard deviations (RSDs) for retention times and peak areas were <0.71% and <6.02%, respectively. The chromatographic fingerprints of four types of tobacco flavors (samples A-D) from five different batches were obtained. Nine tobacco flavor samples from different manufacturers (samples AY1-AY3, BY1-BY2, CY1-CY2, DY1-DY2) were also analyzed to obtain their chromatographic fingerprints. Hierarchical cluster and similarity analyses were used to evaluate the quality of tobacco flavors from different manufacturers. Hierarchical clustering refers to the process of subdividing a group of samples into clusters that exhibit a high degree of intracluster similarity and intercluster dissimilarity. The dendrograms obtained using SPSS 12.0 indicated good quality consistency among the samples in different batches. Samples AY3, BY2, CY2, and DY1 clustered with the batches of standard tobacco flavors. Therefore, hierarchical cluster analysis can effectively distinguish the quality of products from different manufacturers. The Similarity Evaluation System for Chromatographic Fingerprint of Traditional Chinese Medicine (version 2.0) was used to evaluate the similarity between the standard tobacco flavors and products from different manufacturers. Among the samples analyzed, samples AY3, BY2, CY2, and DY1 showed the highest similarity values (>97.7%), which was consistent with the results of the hierarchical cluster analysis. This finding indicates that IC combined with chromatographic fingerprint analysis could accurately determine the quality of tobacco flavors. GC combined with ultrasonic-assisted liquid-liquid extraction was also used to analyze the tobacco flavors and verify the accuracy of the proposed method. Compared with GC coupled with ultrasonic-assisted liquid-liquid extraction, IC demonstrated more significant quality differences among certain tobacco flavors.


Assuntos
Nicotiana , Controle de Qualidade , Nicotiana/química , Aromatizantes/análise , Produtos do Tabaco/análise , Cromatografia Líquida de Alta Pressão/métodos , Cromatografia Gasosa/métodos , Cromatografia por Troca Iônica/métodos
2.
Food Chem ; 455: 139952, 2024 Oct 15.
Artigo em Inglês | MEDLINE | ID: mdl-38850968

RESUMO

Dendrobium officinale Kimura & Migo (D. officinale) has been widely used as Chinese medicine and functional food. In present study, the structural characteristics of anthocyanins in D. officinale were investigated by ultra-performance liquid chromatography with diode array detector (UPLC-DAD) and ultra-performance liquid chromatography-quadrupole-time of flight mass spectrometry (UPLC-Q-TOF-MS/MS). Totally, 14 anthocyanins were detected and identified, and 13 of them were first reported in D. officinale. Results showed that the vast majority of anthocyanins had multi-glycosylated cyanidin core, with variable acylation pattern mainly comprising phenolic acids. The composition and content of anthocyanins in D. officinale stems with different cultivation modes and years have been compared. The anthocyanins showed potent antioxidant activity in terms of radicals scavenging capacity and reducing power, as well as superior α-amylase and α-glucosidase inhibitory activity. The results provided a complete profile of anthocyanins in D. officinale and laid a foundation for further utilizing them as functional foods.


Assuntos
Antocianinas , Antioxidantes , Dendrobium , Hipoglicemiantes , Extratos Vegetais , Antioxidantes/química , Antioxidantes/farmacologia , Dendrobium/química , Antocianinas/química , Antocianinas/farmacologia , Hipoglicemiantes/química , Hipoglicemiantes/farmacologia , Extratos Vegetais/química , Extratos Vegetais/farmacologia , Cromatografia Líquida de Alta Pressão , Acilação , alfa-Amilases/química , alfa-Amilases/antagonistas & inibidores , alfa-Amilases/metabolismo , Espectrometria de Massas em Tandem , Estrutura Molecular , alfa-Glucosidases/química , alfa-Glucosidases/metabolismo , Humanos , Inibidores de Glicosídeo Hidrolases/química , Inibidores de Glicosídeo Hidrolases/farmacologia
3.
J Biomech Eng ; 146(5)2024 05 01.
Artigo em Inglês | MEDLINE | ID: mdl-38376449

RESUMO

The COVID-19 pandemic necessitated mainstream adoption of online and remote learning approaches, which were highly advantageous yet challenging in many ways. The online modality, while teaching biomedical engineering-related topics in the areas of biomechanics, mechanobiology, and biomedical sciences, further added to the complexity faced by the faculty and students. Both the benefits and the challenges have not been explored systematically by juxtaposing experiences and reflections of both the faculty and students. Motivated by this need, we designed and conducted a systematic survey named BIORES-21, targeted toward the broader bio-engineering community. Survey responses and our inferences from survey findings cumulatively offer insight into the role of employed teaching/learning technology and challenges associated with student engagement. Survey data also provided insights on what worked and what did not, potential avenues to address some underlying challenges, and key beneficial aspects such as integration of technology and their role in improving remote teaching/learning experiences. Overall, the data presented summarize the key benefits and challenges of online learning that emerged from the experiences during the pandemic, which is valuable for the continuation of online learning techniques as in-person education operations resumed broadly across institutions, and some form of online learning seems likely to sustain and grow in the near future.


Assuntos
Educação a Distância , Humanos , Fenômenos Biomecânicos , Pandemias , Biofísica , Aprendizagem
4.
J Sep Sci ; 47(1): e2300253, 2024 Jan.
Artigo em Inglês | MEDLINE | ID: mdl-37994289

RESUMO

A method for the determination of five microplastics in agricultural soil was established by double-shot pyrolysis-gas chromatography combined with two-step extraction. First, polycarbonate (PC), polystyrene (PS), polypropylene (PP), and polyethylene (PE) were extracted from soil samples using a mixed solvent of cyclohexanone and p-xylene, and then PE terephthalate was extracted with m-methylphenol. Subsequently, PC and PE terephthalate were analyzed by thermochemolysis, and PE, PP, and PS were investigated by direct pyrolysis at 600°C. The linearity of the method was satisfactory for five microplastics and the correlation coefficients were higher than 0.97 in the respective concentration range. The limits of detection and the limits of quantification were 0.2-10.0 and 0.5-20.0 µg/g, respectively. The method provided recoveries of 75.1%-141.5%, with acceptable repeatability within 20.0%. It was a supplementary method for the existing characterization of microplastics in agricultural soil.

5.
J Hazard Mater ; 464: 133007, 2024 02 15.
Artigo em Inglês | MEDLINE | ID: mdl-37984142

RESUMO

The detection of illicit drugs in wastewater can effectively monitor and evaluate the trend of illicit drug abuse. A novel mixed-mode cation exchange magnetic sorbent Fe3O4 @poly(ST/DVB/MA-COOH) was prepared and firstly applied as magnetically dispersed solid phase extraction material to efficiently, rapidly, and selectively extract 21 illicit drugs from wastewater. The selectivity of the sorbent was mainly attributed to the electrostatic interaction. The effects of Fe3O4 @poly(ST/DVB/MA-COOH) preparation and extraction conditions on the adsorption performance were thoroughly discussed. Among the 21 illicit drugs, the absolute extraction recovery values for 19 illicit drugs were greater than 80 % and the entire adsorption process could be achieved in one minute. Subsequently, the Fe3O4 @poly(ST/DVB/MA-COOH) sorbent combined with UHPLC-MS/MS was used to establish a quantitative method for the effectively extracted 19 illicit drugs in wastewater. The method had a good determination coefficient in the range of 0.2-200 ng/L and the limits of detection of the method were 0.03-0.67 ng/L. The spiked recovery values were in the range of 87.0-119.6 %. Finally, the method was successfully applied to the detection of 19 illicit drugs in wastewater samples and also compared with the commonly used SPE method. The obtained results indicate that Fe3O4 @poly(ST/DVB/MA-COOH) has great advantages in the detection of illicit drugs in wastewater.


Assuntos
Drogas Ilícitas , Poluentes Químicos da Água , Águas Residuárias , Espectrometria de Massas em Tandem/métodos , Extração em Fase Sólida/métodos , Cátions , Fenômenos Magnéticos , Cromatografia Líquida de Alta Pressão/métodos , Poluentes Químicos da Água/análise
6.
J Craniomaxillofac Surg ; 52(2): 234-239, 2024 Feb.
Artigo em Inglês | MEDLINE | ID: mdl-38161074

RESUMO

This study aimed to validate the predictors of speech outcomes following Furlow palatoplasty in patients with velopharyngeal insufficiency (VPI) after primary palatoplasty and to propose and validate a model to predict the risk of persistent VPI. The study included patients with VPI after primary palatoplasty who underwent Furlow palatoplasty as a secondary surgery. Eleven variables were included: velar length, pharyngeal cavity depth, velopharyngeal gap, velopharyngeal closure pattern, sex, presence of cleft lip, existence of palatal fistula, surgeon, age at primary palatoplasty, age at secondary surgery, and time interval between primary palatoplasty and secondary surgery. Postoperative speech outcomes were assessed at least 1 year after the secondary surgery and classified as velopharyngeal competence (VPC) or VPI. Variables were analyzed using multivariate logistic regression analysis, and the area under the curve (AUC) was used to validate model accuracy. The study sample comprised 101 patients. Of the patients, 62 had VPC and 39 had VPI after secondary surgery. The results showed a younger age at secondary surgery, a smaller velopharyngeal gap, being female, having a coronal velopharyngeal closure pattern and a velopharyngeal closure ratio of 90% or greater produced a greater probability of VPC. Given the constraints of this study, it appears that the Furlow palatoplasty should be prioritized when the clinical model predicts a substantial likelihood of VPC post-surgery.


Assuntos
Fissura Palatina , Insuficiência Velofaríngea , Humanos , Feminino , Masculino , Insuficiência Velofaríngea/etiologia , Insuficiência Velofaríngea/cirurgia , Fala , Palato Mole/cirurgia , Resultado do Tratamento , Fissura Palatina/cirurgia , Fissura Palatina/complicações , Estudos Retrospectivos
7.
J Chromatogr A ; 1710: 464415, 2023 Nov 08.
Artigo em Inglês | MEDLINE | ID: mdl-37783003

RESUMO

Hollow fiber-solid phase microextraction combined with micro sample collector assisted injection technique was developed for the detection of trace fatty acid methyl esters in biodiesel wastewater. Polypropylene hollow fiber was employed as extraction material to absorb fatty acid methyl esters in biodiesel wastewater. After the adsorption, hollow fiber was sleeved on the needle core of a micro sample collector and introduced directly into a GC injector for thermal desorption of the analytes. The selectivity of polypropylene hollow fiber on fatty acid methyl esters was investigated by extracting common pollutants in wastewater. Under the optimal conditions, the enrichment factors of polypropylene hollow fiber for methyl palmitate, methyl linoleate, methyl oleate, and methyl stearate were tested as high as 471, 287, 527, and 801, respectively. The quantitative method was validated and the linearity was satisfactory over a concentration range of 10-2000 µg/L with the correlation coefficients more than 0.9990 for 4 fatty acid methyl esters. The limits of detection and quantification were 0.04-0.40 µg/L and 10.0 µg/L, respectively. The recoveries were in the range of 92.0-116.7% by analyzing actual spiked samples. The results showed that the established method was suitable for the analysis of trace fatty acid methyl esters in water samples, with simple operation, low cost and environmental friendliness.


Assuntos
Microextração em Fase Sólida , Águas Residuárias , Microextração em Fase Sólida/métodos , Biocombustíveis , Polipropilenos , Adsorção
8.
Food Chem ; 428: 136819, 2023 Dec 01.
Artigo em Inglês | MEDLINE | ID: mdl-37437357

RESUMO

The structure characteristics, functional properties, antioxidant and hypoglycemic activities of pectins extracted from feijoa peel with water (FP-W), acid (FP-A) and alkali (FP-B) were investigated. Results showed that the feijoa peel pectins (FPs) were mainly composed of galacturonic acid, arabinose, galactose and rhamnose. FP-W and FP-A had higher proportion of homogalacturonan domain, degree of esterification and molecular weight (for main component) than FP-B; FP-B owned the highest yield, protein and polyphenol contents. FP-W had a compact and smooth surface morphology unlike FP-A and FP-B. FP-W and FP-A had better thermal stability than FP-B. The rheological analysis suggested that the FPs exhibited pseudoplastic fluid behavior, and the elastic characteristics were dominant. Results showed that FP-W and FP-B had superior antioxidant and hypoglycemic activities than FP-A. According to correlation analysis, monosaccharide composition, sugar ratios and degree of acetylation were chief factors affecting the functional properties, antioxidant and hypoglycemic activities of the FPs.


Assuntos
Antioxidantes , Feijoa , Antioxidantes/farmacologia , Antioxidantes/química , Pectinas/química , Peso Molecular , Galactose/química
9.
J Chromatogr A ; 1690: 463778, 2023 Feb 08.
Artigo em Inglês | MEDLINE | ID: mdl-36640680

RESUMO

A method for the determination of polyvinyl chloride was developed by the use of a micro sample pretreatment technique combined with ion chromatography. Polyvinyl chloride sample was placed in a sealed glass capillary containing 10 µL deionized water. As a micro pyrolysis reactor, the sealed glass capillary was maintained at 300 °C for 2 min in an oven. Under the above temperature, polyvinyl chloride was pyrolyzed rapidly and released hydrogen chloride, which was easily absorbed by deionized water. Subsequently, the absorption liquid was transferred to a volumetric flask and diluted to 10 mL. Ion chromatography was utilized to detect the content of chloride ion in the diluted absorption liquid for the quantification of polyvinyl chloride in samples. Good linear correlation coefficient (r = 0.9999) was obtained over a range of 0.02-2.00 mg polyvinyl chloride. Appropriate precision with the relative standard deviation below 16.4% and good recoveries between 86.0 and 119.4% were achieved in this work. The limits of detection and quantification were 0.004 mg and 0.012 mg for polyvinyl chloride respectively. The contents of polyvinyl chloride in real samples determined by the micro sample pretreatment technique were consistent with the results obtained by the referenced oxygen flask combustion method. It proved that the proposed method is simple, rapid and accurate for the determination of polyvinyl chloride in real samples.


Assuntos
Cromatografia , Cloreto de Polivinila , Cloreto de Polivinila/química , Água , Cromatografia Líquida de Alta Pressão/métodos
10.
Front Pharmacol ; 13: 1014173, 2022.
Artigo em Inglês | MEDLINE | ID: mdl-36210805

RESUMO

Natural alkaloids are polycyclic, nitrogen-containing, and basic compounds obtained from plants. In this review, the advances in bioactive alkaloids with respect to their chemical structures, herbal sources, and effects for the prevention and treatment of osteoporosis are discussed. Anti-osteoporosis alkaloids are classified into six categories based on the chemical structure, namely, isoquinoline alkaloids, quinolizidine alkaloids, piperidine alkaloids, indole alkaloids, pyrrolizidine alkaloids and steroidal alkaloids. They promote mesenchymal stem cells differentiation, improve osteoblast proliferation, stimulate osteoblast autophagy and suppress osteoclast formation. These natural alkaloids can regulate multiple signaling pathways, including interrupting the tumor necrosis factor receptor associated factor 6- receptor activator of nuclear factor kappa B interaction, inhibiting the nuclear factor kappa B pathway in osteoclasts, activating the p38 mitogen-activated protein kinases pathway in osteoblasts, and triggering the wingless and int-1 pathway in mesenchymal stem cells. This review provides evidence and support for novel drug and clinical treatment of osteoporosis using natural alkaloids.

11.
J Chromatogr A ; 1671: 462994, 2022 May 24.
Artigo em Inglês | MEDLINE | ID: mdl-35378320

RESUMO

A novel mixed-mode weak cation-exchange sorbent (PS-DVB-WCX-II) was prepared by the modification of polystyrene-divinylbenzene with mercaptosuccinic acid for the selective extraction of illicit drugs in environmental water. The PS-DVB-WCX-II was synthesized through the Friedel-Crafts acylation reaction on the surface of polystyrene-divinylbenzene, followed by nucleophilic substitution reaction and thiol-ene click reaction. The sorbent can selectively absorb illicit drugs through the reverse-phase interactions provided by benzene ring on the polymer backbone and the ion-exchange interactions provided by functional group (-COOH). As compared with the extraction performance of three commercial SPE cartridges, it was found that the prepared sorbent had better adsorption performance with the recovery values between 84.1% and 106.0% for the selected 11 illicit drugs under the optimized SPE conditions. Illicit drugs in environmental water were extracted by the sorbent, prior to the detection of UHPLC-MS/MS. Two quantitative methods were established respectively for the detection of 11 illicit drugs in different matrices of river water and wastewater. Both methods had good determination coefficient (r2>0.992) in the range of 0.5-50 ng/L, 2.5-250 ng/L, 5-500 ng/L, and low limits of detection (S/N = 3) of 0.17-1.67 ng/L. In the real wastewater samples, the concentration of morphine was 18.3-126.3 ng/L, and the methamphetamine was 12.7-27.4 ng/L. Meanwhile, PS-DVB-WCX-II was compared with Oasis MCX and Oasis HLB in the detection of real wastewater samples. The results revealed that PS-DVB-WCX-II and Oasis MCX had better performance in absorbing methamphetamine than Oasis HLB, and PS-DVB-WCX-II had better ability to remove the matrix. The results suggested that the prepared weak cation-exchange sorbent had the potential in the application of illicit drug detection in environmental water.


Assuntos
Drogas Ilícitas , Metanfetamina , Poluentes Químicos da Água , Cátions , Poliestirenos , Extração em Fase Sólida/métodos , Espectrometria de Massas em Tandem/métodos , Compostos de Vinila , Águas Residuárias , Água/análise , Poluentes Químicos da Água/análise
12.
China CDC Wkly ; 3(36): 751-756, 2021 Sep 03.
Artigo em Inglês | MEDLINE | ID: mdl-34594983

RESUMO

WHAT IS KNOWN ABOUT THIS TOPIC?: The emerging H5Ny lineages of the avian influenza virus (AIV) with genomic reassortments have posed a continuous threat to animals and human beings. Since the first case of avian influenza A (H5N6) virus infection in 2014, the World Health Organization has reported a total of 38 cases by August 6, 2021. WHAT IS ADDED BY THIS REPORT?: A total of 5 new cases of H5N6 that occurred from May 2021 to July 2021 in Sichuan Province, China were reported in this study. Epidemiological and laboratory information of the five cases were investigated. The genomic analysis of the H5N6 genomes showed the features of AIV genomic reassortments and key residue substitutions. WHAT ARE THE IMPLICATIONS FOR PUBLIC HEALTH PRACTICE?: The emergence of human cases infected by AIV H5Ny lineages through time demonstrates a risk of the persistence and evolution of the virus to trigger sporadic outbreaks and even pandemics, which need continuous surveillance.

13.
PLoS One ; 16(4): e0250717, 2021.
Artigo em Inglês | MEDLINE | ID: mdl-33901236

RESUMO

BACKGROUND: Ovarian cancer (OC) is a leading cause of death in gynecological malignancies worldwide. Multitudinous studies have suggested the potential of circulating tumor DNA (ctDNA), circulating microRNAs (miRNAs), and long non-coding RNAs (lncRNAs) as novel diagnostic molecular biomarkers for OC. Here, we include three updated meta-analysis methods using different molecular biomarkers to evaluate their discriminative value in OC diagnosis. METHODS: We conducted three meta-analyses after searching different databases, and 23 eligible articles, including 8 concerning ctDNA, 11 concerning miRNAs, and 4 concerning lncRNAs, were found. Further, we pooled data concerning the sensitivity, specificity, and other indicators of accuracy for ctDNA/miRNAs/lncRNAs in the diagnosis of OC. The heterogeneity was further explored by meta-regressions and subgroup analyses, and Deeks' funnel plots were used to measure the publication bias of these three meta-analyses. RESULTS: In all, this meta-analysis included 1732 OC patients and 3958 controls. The sensitivity of ctDNA for OC diagnosis was superior to that of lncRNA and miRNA (84% vs. 81% vs. 78%). Moreover, the specificity and area under the receiver-operating characteristic (ROC) curve (AUC) of ctDNA were 91% and 94%, which were significantly higher than those of miRNA and lncRNAs (78% and 85%; 78% and 86%, respectively). No significant difference was observed among the two meta-analyses of ctDNA and lncRNA (P > 0.05) with regard to publication bias, while the meta-analysis of miRNA observed a significantly small publication bias (P < 0.05). CONCLUSION: ctDNA/miRNAs/lncRNAs may be promising molecular biomarkers for OC diagnosis. Further large-scale studies are needed to verify the potential applicability of ctDNA/miRNAs/lncRNAs molecular signatures alone or in combination as diagnostic molecular biomarkers for OC.


Assuntos
Biomarcadores Tumorais/genética , DNA Tumoral Circulante/sangue , MicroRNAs/sangue , Neoplasias Ovarianas/diagnóstico , RNA Longo não Codificante/sangue , Área Sob a Curva , Biomarcadores Tumorais/sangue , Feminino , Humanos , Neoplasias Ovarianas/genética , Curva ROC , Sensibilidade e Especificidade
14.
J Sep Sci ; 44(9): 1913-1922, 2021 May.
Artigo em Inglês | MEDLINE | ID: mdl-33665927

RESUMO

In this study, a peptide-based method employing ultra high performance liquid chromatography electrostatic field orbitrap high-resolution mass spectrometry and triple quadrupole mass spectrometry was developed for quantification of A1-type and A2-type ß-casein in milk from Yak, cows, and their offspring of crosses, Pien-niu. The specific peptides of A1-type and A2-type ß-casein were screened and confirmed by protein software after analysis of high-resolution mass spectrometry. The multiple reaction monitoring method was established based on the qualitative results, and isotope-label peptides were used as internal standards. The linear correlation coefficients of this method were >0.99. The relative standard deviations of repeatability test were 0.2-3.6%. The recovery rate ranged from 93.3 to 114.4% with relative standard deviations <6% at three different spiking levels. The method was applied to analyze 45 milk samples from different species. The results showed that ß-casein in Yak and Pien-niu milk was about 30% higher than that in cow milk. Furthermore, the ß-casein in the Yak milk only contains A2-type ß-casein. A1-type and A2-type ß-casein coexist in most samples of Pien-niu and cow milk, a few samples contain only one type of ß-casein. These results provide further understanding in nutritional value of milk from Yak and Pien-niu.


Assuntos
Caseínas/análise , Leite/química , Animais , Bovinos , Cromatografia Líquida de Alta Pressão , Espectrometria de Massas , Peptídeos/química
15.
J Pharm Biomed Anal ; 193: 113723, 2021 Jan 30.
Artigo em Inglês | MEDLINE | ID: mdl-33166839

RESUMO

To explore the MS fragmentation pattern of synthetic cannabinoids by electrospray ionization mass spectrometry, twenty-seven synthetic cannabinoids were systematically investigated by liquid chromatography coupled to high-resolution quadrupole Orbitrap mass spectrometry(LC-Q-Orbitrap/MS)with positive mode of electrospray ionization. Based on tandem multistage MS and high resolution MS data, MS fragmentation pattern of synthetic cannabinoids was summarized. The cleavage of CC bonds next to the oxygen at the side chain on the C-3 position of synthetic cannabinoids was the characteristic fragmentation pathway of synthetic cannabinoids in the positive mode of electrospray ionization. When the synthetic cannabinoids with a 3-carbamoylpropyl-indole/indazole structure, NH3, CO, NH2CHO and CH2(CH3)2 were easy to lose to form different ions. While when the synthetic cannabinoids with a 3-carboxamide-indole/indazole structure, the side chain on the C-3 position was susceptible to γ-cleavage. In addition, this MS fragmentation pattern was applied to quickly screen whether electronic cigarette oil and tobacco from drug cases contain synthetic cannabinoids. This kind of compounds had strong fragmentation pattern, which provided new evidence for the rapid structure identification of synthetic cannabinoids.


Assuntos
Canabinoides , Sistemas Eletrônicos de Liberação de Nicotina , Cromatografia Líquida , Íons , Espectrometria de Massas por Ionização por Electrospray
16.
Artigo em Inglês | MEDLINE | ID: mdl-32738526

RESUMO

A rapid and sensitive method utilizing flash evaporation-gas chromatography/mass spectrometry (FE-GC/MS) has been developed. The method is applicable to determine ketamine (KET), methamphetamine (MAMP) and 3,4-methylenedioxymethamphetamine (MDMA) in human hair. Cut and weighted hair (0.30 mg) was heated at the flash evaporation temperature of 350 °C. KET, MAMP and MDMA were released into a capillary column for GC/MS analysis and produced fragment ions in SIM mode. Validation of the method included evaluation of linearity, sensitivity, accuracy, precision and repeatability. Linearity ranged from 2 to 300 ng/mg for KET in hair and 2 to 200 ng/mg for MAMP and MDMA in hair with the correlation coefficients all greater than 0.998. Limits of detection were 0.7 ng/mg and limits of quantification were 2.0 ng/mg of hair for KET, MAMP and MDMA. The precision ranged from 1.57% to 7.75% for KET, 1.49% to 7.10% for MAMP and 1.84% to 8.31% for MDMA. The recovery ranged from 102.1% to 110.9% for KET, 99.3% to 108.0% for MAMP and 89.5% to 112.6% for MDMA. Six authentic hair samples from known drug abusers and three drug-free hair samples from volunteers who had never used drugs were successfully analyzed. Compared with traditional time-consuming and hair-comsuming pretreatment method, FE-GC/MS was a faster, simpler and low sample consumption method for the determination of KET, MAMP and MDMA in human hair.


Assuntos
Cromatografia Gasosa-Espectrometria de Massas/métodos , Cabelo/química , Ketamina/análise , Metanfetamina/análise , N-Metil-3,4-Metilenodioxianfetamina/análise , Humanos , Limite de Detecção , Modelos Lineares , Reprodutibilidade dos Testes , Detecção do Abuso de Substâncias
17.
J Chromatogr A ; 1619: 460953, 2020 May 24.
Artigo em Inglês | MEDLINE | ID: mdl-32178861

RESUMO

A solid phase microextraction coupled with flash evaporation gas chromatography method was applied to the determination of phthalate esters (PAEs). Polysulfone (PSF) hollow fiber at 1 cm length was employed as extraction element to adsorb PAEs directly. Predominant parameters including stirring velocity, salt concentration, extraction time and extraction temperature were optimized. PSF fiber with absorbed PAEs was put into a small sample cup. The extracted analytes were thermally desorbed at 300 °C in a pyrolyzer, and then entered into a column for separation. The linearity of the method was satisfactory over a concentration range of 2-1000 µg/L with the correlation coefficients r>0.99 for all analytes except dimethoxyethyl phthalate. The relative standard deviations for peak areas were below 9.5% (n = 6). The developed technique achieved high enrichment factors (280-9930 times) and low limits of detection (0.001-0.130 µg/L). The recoveries over the range of 87.0-117.7% were obtained by analyzing real spiked samples. The results demonstrated that this was a simple, environmentally friendly and accurate method for the determination of PAEs in bottled water samples.


Assuntos
Cromatografia Gasosa , Água Potável/química , Ésteres/isolamento & purificação , Ionização de Chama , Análise de Alimentos/métodos , Polímeros/química , Microextração em Fase Sólida , Sulfonas/química , Adsorção , Ésteres/análise , Ácidos Ftálicos/isolamento & purificação , Temperatura
18.
Bioorg Med Chem ; 28(5): 115229, 2020 03 01.
Artigo em Inglês | MEDLINE | ID: mdl-32033878

RESUMO

Many human diseases, including cystic fibrosis lung infections, are caused or exacerbated by bacterial biofilms. Specialized modes of motility, including swarming and twitching, allow gram-negative bacteria to spread across surfaces and form biofilms. Compounds that inhibit these motilities could slow the spread of biofilms, thereby allowing antibiotics to work better. We previously demonstrated that a set of plant-derived triterpenes, including oleanolic acid and ursolic acid, inhibit formation of Escherichia coli and Pseudomonas aeruginosa biofilms, and alter expression of genes involved in chemotaxis and motility. In the present study, we have prepared a series of analogs of oleanolic acid. The analogs were evaluated against clinical isolates of E. coli and P. aeruginosa in biofilm formation assays and swarming assays. From these analogs, compound 9 was selected as a lead compound for further development. Compound 9 inhibits E. coli biofilm formation at 4 µg/mL; it also inhibits swarming at ≤1 µg/mL across multiple clinical isolates of P. aeruginosa, E. coli, Burkholderia cepacia, and Salmonella enterica, and at <0.5 µg/mL against multiple agricultural strains. Compound 9 also potentiates the activity of the antibiotics tobramycin and colistin against swarming P. aeruginosa; this is notable, as tobramycin and colistin are inhaled antibiotics commonly used to treat P. aeruginosa lung infections in people with cystic fibrosis. qPCR experiments suggested that 9 alters expression of genes involved in regulating Type IV pili; western blots confirmed that expression of Type IV pili components PilA and PilY1 decreases in P. aeruginosa in the presence of 9.


Assuntos
Aminas/farmacologia , Antibacterianos/farmacologia , Biofilmes/efeitos dos fármacos , Bactérias Gram-Negativas/efeitos dos fármacos , Aminas/síntese química , Aminas/química , Antibacterianos/síntese química , Antibacterianos/química , Relação Dose-Resposta a Droga , Testes de Sensibilidade Microbiana , Estrutura Molecular , Relação Estrutura-Atividade
19.
J Chromatogr A ; 1601: 104-114, 2019 Sep 13.
Artigo em Inglês | MEDLINE | ID: mdl-31227360

RESUMO

In this work, a simple sugaring-out assisted liquid-liquid extraction (SULLE) method coupled with high performance liquid chromatography-electrochemical detection (HPLC-ECD) has been developed for rapid and sensitive determination of 17 phenolic compounds in honey. To achieve the maximum extraction efficiency of target analytes, several parameters, such as pH, ionic strength, extraction times and the volume of extracting solvent were optimized. Chromatographic separation was performed on a C18 column with a gradient methanol/aqueous formic acid elution, and the ECD was set at 1.0 V in oxidative mode. Under the optimal conditions, good linearity was obtained for 17 phenolic compounds with the coefficients of determination (R2) higher than 0.9986 in the range of 0.05-20 µg mL-1. The limits of detection (LODs, S/N = 3) for the 17 phenolic compounds were in the range of 0.20-1.26 µg kg-1 by ECD, 9-83 times lower than those obtained with UV detection. Satisfactory recoveries between 79.8% and 105.7% were obtained for spiked honey samples with relative standard deviations (RSD) less than 5.1%. Compared with conventional LLE method, the proposed SULLE method provided higher extraction efficiency and had advantages of rapidity, ease of operation, much less consumption of organic solvents and samples. The proposed HPLC-ECD method featuring excellent sensitivity and selectivity has been applied to the quantification of phenolic compounds in honey samples of different floral origin.


Assuntos
Cromatografia Líquida de Alta Pressão , Técnicas Eletroquímicas , Análise de Alimentos/métodos , Mel/análise , Extração Líquido-Líquido , Fenóis/análise , Açúcares/química , Limite de Detecção , Solventes/química
20.
Spectrochim Acta A Mol Biomol Spectrosc ; 213: 210-217, 2019 Apr 15.
Artigo em Inglês | MEDLINE | ID: mdl-30690304

RESUMO

The present paper reported a hybrid structure for the optical recognition of PA (picric acid). This dye-MOF structure, named as R6h@EuBTC, consisted of a supporting matrix based on rare earth MOF and a sensing probe based on rhodamine dye, which was confirmed using XRD, IR, thermal and photophysical analysis. R6h@EuBTC's rhodamine absorption in visible region was enhanced by increasing PA concentrations, showing obvious color change and consequently colorimetric sensing. R6h@EuBTC's rhodamine emission component was increased by increasing PA concentrations, while its Eu emission component was slightly quenched by increasing PA concentrations, which offered self-calibrated sensing signals for ratiometric fluorescent sensing. Linear response and good selectivity were observed for both sensing channels with LOD of 3.9 µM. R6h@EuBTC's sensing mechanism towards PA was the combination of two procedures, which were the emission turn on effect of rhodamine component triggered by PA-released protons and the emission turn off effect of Eu component caused by its electron transfer procedure to PA, respectively. R6h@EuBTC's novelty was its two sensing channels and the practicability of naked eye detection.

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