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1.
Anim Sci J ; 95(1): e13952, 2024.
Artigo em Inglês | MEDLINE | ID: mdl-38689465

RESUMO

Defatted Lagenaria siceraria seed flour (DLSSF) was obtained from defatted seed cake, dried, and ground through a sieve of 500 µm and characterized. A 2 × 4 factorial design (two flour hydration rates and four fat substitution rates) was used to produce a low-fat beef patty by replacing fat with DLSSF. Beef kidney fat was used to formulate the control sample. Chemical, physical, technological, sensory, and nutritional characteristics of low-fat beef patties manufactured were evaluated. DLSSF contains mainly protein. As fat replacers, DLSSF induces a significant increase in the pH of the raw and cooked patty, the moisture and protein contents, the cooking yield, the cohesion, chewiness, springiness, and lightness of the cooked beef patty with fat substitution rate. There is a decrease in fat content, total calories, water retention capacity, hardness, and redness of the cooked patty with a fat substitution rate. From the sensory analysis, the substitution of fat improves the acceptability of samples. Based on the overall parameters analyzed, DLSSF containing 60% water can be used to produce low-fat beef patty by replacing fat at 100%. From these results, hydrated DLSSF could be an effective method to solve the problems of noncommunicable diseases related to animal fat consumption.


Assuntos
Fenômenos Químicos , Culinária , Farinha , Sementes , Sementes/química , Animais , Bovinos , Culinária/métodos , Farinha/análise , Substitutos da Gordura/análise , Cucurbitaceae/química , Produtos da Carne/análise , Humanos , Água/análise , Qualidade dos Alimentos , Concentração de Íons de Hidrogênio , Paladar , Valor Nutritivo
2.
Geobiology ; 22(3): e12600, 2024.
Artigo em Inglês | MEDLINE | ID: mdl-38725144

RESUMO

Microbial sulfate reduction is central to the global carbon cycle and the redox evolution of Earth's surface. Tracking the activity of sulfate reducing microorganisms over space and time relies on a nuanced understanding of stable sulfur isotope fractionation in the context of the biochemical machinery of the metabolism. Here, we link the magnitude of stable sulfur isotopic fractionation to proteomic and metabolite profiles under different cellular energetic regimes. When energy availability is limited, cell-specific sulfate respiration rates and net sulfur isotope fractionation inversely covary. Beyond net S isotope fractionation values, we also quantified shifts in protein expression, abundances and isotopic composition of intracellular S metabolites, and lipid structures and lipid/water H isotope fractionation values. These coupled approaches reveal which protein abundances shift directly as a function of energy flux, those that vary minimally, and those that may vary independent of energy flux and likely do not contribute to shifts in S-isotope fractionation. By coupling the bulk S-isotope observations with quantitative proteomics, we provide novel constraints for metabolic isotope models. Together, these results lay the foundation for more predictive metabolic fractionation models, alongside interpretations of environmental sulfur and sulfate reducer lipid-H isotope data.


Assuntos
Desulfovibrio vulgaris , Proteômica , Isótopos de Enxofre , Isótopos de Enxofre/análise , Isótopos de Enxofre/metabolismo , Desulfovibrio vulgaris/metabolismo , Proteoma/metabolismo , Proteoma/análise , Metabolismo Energético , Metaboloma , Proteínas de Bactérias/metabolismo , Oxirredução , Sulfatos/metabolismo
3.
J Mass Spectrom ; 59(6): e5031, 2024 Jun.
Artigo em Inglês | MEDLINE | ID: mdl-38726684

RESUMO

Managing ocular microbial infections typically requires pharmacotherapy using antibiotic eye drops, such as moxifloxacin hydrochloride (MFX), combined with an antifungal agent like amphotericin B (AB). We carried out and validated an LC-MS/MS assay to quantify these compounds in rabbit tear fluid in order to look into the pharmacokinetics of these two drugs. We employed a protein precipitation technique for the extraction of drugs under examination. A Waters Symmetry C18 column was used to separate the analytes and internal standard. The composition of the mobile phase was like (A) 0.1% v/v formic acid in water and (B) methanol. The detection of MFX and AB was accomplished through the utilization of positive ion electrospray ionization under multiple reaction monitoring mode. The linearity curves for both analytes exhibited an acceptable trendline across a concentration range of 2.34-300 ng/mL for MFX and 7.81-1000 ng/mL for AB in surrogate rabbit tear fluid. The lower limit of quantitation for MFX was 2.34 ng/mL, while for AB, it was 7.81 ng/mL. The approach was strictly validated, encompassing tests of selectivity, linearity (with r2 > 0.99), precision, accuracy, matrix effects, and stability. Consequently, we employed this method to evaluate the pharmacokinetics profiles of MFX and AB in rabbit tear fluid following single topical doses.


Assuntos
Moxifloxacina , Espectrometria de Massas em Tandem , Lágrimas , Coelhos , Animais , Espectrometria de Massas em Tandem/métodos , Lágrimas/química , Moxifloxacina/farmacocinética , Moxifloxacina/análise , Reprodutibilidade dos Testes , Anfotericina B/farmacocinética , Anfotericina B/análise , Limite de Detecção , Anti-Infecciosos/farmacocinética , Anti-Infecciosos/análise , Cromatografia Líquida/métodos , Soluções Oftálmicas/farmacocinética , Modelos Lineares , Espectrometria de Massa com Cromatografia Líquida
4.
J Mass Spectrom ; 59(6): e5036, 2024 Jun.
Artigo em Inglês | MEDLINE | ID: mdl-38726689

RESUMO

Turmeric and ginger are extensively employed as functional ingredients due to their high content of curcuminoids and gingerols, considered the key bioactive compounds found in these roots. In this study, we present an innovative and fast method for the assay of curcuminoids and gingerols in different foods containing the two spices, with the aim of monitoring the quality of products from a nutraceutical perspective. The proposed approach is based on paper spray tandem mass spectrometry coupled with the use of a labeled internal standard, which has permitted to achieve the best results in terms of specificity and accuracy. All the calculated analytical parameters were satisfactory; accuracy values are around 100% for all spiked samples and the precision data result lower than 15%. The protocol was applied to several real samples, and to demonstrate its robustness and reliability, the results were compared to those arising from the common liquid chromatographic method.


Assuntos
Curcuma , Álcoois Graxos , Espectrometria de Massas em Tandem , Zingiber officinale , Zingiber officinale/química , Curcuma/química , Espectrometria de Massas em Tandem/métodos , Álcoois Graxos/análise , Reprodutibilidade dos Testes , Limite de Detecção , Catecóis/análise , Análise de Alimentos/métodos , Curcumina/análise , Curcumina/análogos & derivados , Papel
5.
J Mass Spectrom ; 59(6): e5033, 2024 Jun.
Artigo em Inglês | MEDLINE | ID: mdl-38726726

RESUMO

A total of 43 compounds, including phenolic acids, flavonoids, lignans, and diterpene, were identified and characterized using UPLC-ESI-Q-TOF-MS coupled with UNIFI software. The identified flavonoids were mostly isomers of luteolin, apigenin, and quercetin, which were elucidated and distinguished for the first time in pepper cultivars. The use of multivariate data analytics for sample discrimination revealed that luteolin derivatives played the most important role in differentiating pepper cultivars. The content of phenolic acids and flavonoids in immature green peppers was generally higher than that of mature red peppers. The pepper extracts possessed significant antioxidant activities, and the antioxidant activities correlated well with phenolic contents and their molecular structure. In conclusion, the findings expand our understanding of the phytochemical components of the Chinese pepper genotype at two maturity stages. Moreover, a UPLC-ESI-Q-TOF-MS in negative ionization mode rapid methods for characterization and isomers differentiation was described.


Assuntos
Antioxidantes , Capsicum , Fenóis , Espectrometria de Massas por Ionização por Electrospray , Espectrometria de Massas por Ionização por Electrospray/métodos , Antioxidantes/química , Antioxidantes/análise , Antioxidantes/farmacologia , Cromatografia Líquida de Alta Pressão/métodos , Capsicum/química , Isomerismo , Fenóis/química , Fenóis/análise , Flavonoides/química , Flavonoides/análise , Extratos Vegetais/química , População do Leste Asiático
6.
J Mass Spectrom ; 59(6): e5035, 2024 Jun.
Artigo em Inglês | MEDLINE | ID: mdl-38726730

RESUMO

Bupleuri Radix is an important medicinal plant, which has been used in China and other Asian countries for thousands of years. Cultivated Bupleurum chinense DC. (B. chinense) is the main commodity of Bupleuri Radix. The benefits of intercropping with various crops for B. chinense have been recognized; however, the influence of intercropping on the chemical composition of B. chinense is still unclear yet. In this study, intercropping with sorghum and maize exhibited little effect on the root length, root diameter, and single root mass of B. chinense. Only the intercropping with sorghum increased the root length of B. chinense slightly compared to the monocropping. In addition, 200 compounds were identified by UHPLC-Q-TOF-MS, and metabolomic combined with the Venn diagram and heatmap analysis showed apparent separation between the intercropped and monocropped B. chinense samples. Intercropping with sorghum and maize could both increase the saikosaponins, fatty acyls, and organic acids in B. chinense while decreasing the phospholipids. The influence of intercropping on the saikosaponin biosynthesis was probably related with the light intensity and hormone levels in B. chinense. Moreover, we found intercropping increased the anti-inflammatory activity of B. chinense. This study provides a scientific reference for the beneficial effect of intercropping mode of B. chinense.


Assuntos
Bupleurum , Metabolômica , Ácido Oleanólico , Raízes de Plantas , Saponinas , Sorghum , Zea mays , Sorghum/metabolismo , Sorghum/química , Bupleurum/química , Bupleurum/metabolismo , Zea mays/metabolismo , Zea mays/química , Saponinas/análise , Saponinas/metabolismo , Ácido Oleanólico/análogos & derivados , Ácido Oleanólico/análise , Ácido Oleanólico/metabolismo , Metabolômica/métodos , Cromatografia Líquida de Alta Pressão/métodos , Raízes de Plantas/metabolismo , Raízes de Plantas/química , Espectrometria de Massas/métodos , Agricultura/métodos , Espectrometria de Massa com Cromatografia Líquida
7.
J Sep Sci ; 47(9-10): e2300867, 2024 May.
Artigo em Inglês | MEDLINE | ID: mdl-38726736

RESUMO

Shengxian decoction, a traditional Chinese medicinal prescription, has been shown to alleviate doxorubicin-induced chronic heart failure. This study established an ultra-performance liquid chromatography-quadrupole time-of-flight mass spectrometry method to separate and characterize the complex chemical compositions of Shengxian decoction, and the absorbed compounds in the bio-samples of the cardiotoxicity rats with chronic heart failure after its oral delivery. Note that 116 chemical compounds were identified from Shengxian decoction in vitro, 81 more than previously detected. Based on the three-dimensional data of these compounds, 28 absorbed compounds were confirmed in vivo. Network pharmacology and molecular docking experiments indicated that timosaponin B-II, timosaponin A-III, gitogenin, and 7,8-didehydrocimigenol were recognized as the key effective compounds to exert effects against doxorubicin cardiotoxicity by acting on targets such as caspase 3, cyclin-dependent kinase 1, cyclin-dependent kinase 4, receptor tyrosine-protein kinase erbB-2, and mitogen-activated protein kinase 1 in p53 and phosphatidylinositol 3-kinase-Akt signaling pathways. This study developed the understanding of the composition of Shengxian decoction for the treatment of doxorubicin cardiotoxicity, as well as a feasible strategy to elucidate the effective constituents in traditional Chinese medicines.


Assuntos
Doxorrubicina , Medicamentos de Ervas Chinesas , Farmacologia em Rede , Ratos Sprague-Dawley , Medicamentos de Ervas Chinesas/química , Medicamentos de Ervas Chinesas/farmacologia , Medicamentos de Ervas Chinesas/análise , Animais , Ratos , Cromatografia Líquida de Alta Pressão , Masculino , Espectrometria de Massas , Cardiotoxicidade , Simulação de Acoplamento Molecular , Combinação de Medicamentos
8.
J Sep Sci ; 47(9-10): e2400142, 2024 May.
Artigo em Inglês | MEDLINE | ID: mdl-38726732

RESUMO

Catechins, renowned for their antioxidant properties and health benefits, are commonly present in beverages, particularly tea and wine. An efficient and cost-effective salting-out assisted liquid-liquid extraction (SALLE) method has been developed and validated for the simultaneous determination of six catechins and caffeine in tea and wine samples using high-performance liquid chromatography-ultraviolet (HPLC-UV). This method demonstrates outstanding performance: linearity (1-120 µg/mL, r2 > 0.999), accuracy (96.5%-103.4% recovery), and precision (≤14.7% relative standard deviation), meeting validation requirements set by the US Food and Drug Administration. The reduced sample size (0.1 g) minimizes matrix interferences and costs without compromising sensitivity. All analytes were detected in Camellia sinensis teas, with green tea displaying the highest total catechin content (47.5-100.1 mg/mL), followed by white and black teas. Analysis of wine samples reveals the presence of catechin in all red and white wines, and epigallocatechin gallate in all red wine samples, highlighting the impact of winemaking processes on catechin content. The SALLE-HPLC-UV approach represents a green alternative by eliminating organic waste, surpassing conventional dilution methods in specificity and sensitivity for catechin determination. AGREEprep assessment emphasizes the strengths of the SALLE procedure, including material reusability, throughput efficiency, minimal sample requirements, low energy consumption, and the absence of organic waste generation.


Assuntos
Cafeína , Catequina , Extração Líquido-Líquido , Chá , Vinho , Cromatografia Líquida de Alta Pressão/métodos , Vinho/análise , Cafeína/análise , Catequina/análise , Chá/química , Extração Líquido-Líquido/métodos , Espectrofotometria Ultravioleta , Raios Ultravioleta
9.
J Sep Sci ; 47(9-10): e2300949, 2024 May.
Artigo em Inglês | MEDLINE | ID: mdl-38726739

RESUMO

Hydrophilic interaction liquid chromatography (HILIC) has been widely applied to challenging analysis in biomedical and pharmaceutical fields, bridging the gap between normal-phase high-performance liquid chromatography and reversed-phase high-performance liquid chromatography (RP-HPLC). This paper comprehensively explores the retention mechanisms of amitriptyline and its impurities A, B, C, D, F, and G on amide, amino, diol, and silica columns. Dual HILIC/RP-HPLC retention mechanisms were developed, and transitional points between HILIC and RP-HPLC mechanisms were calculated on amide, diol, and silica columns. Adsorption and partition contributions to overall retention mechanisms were evaluated using Python software in HILIC and RP-HPLC regions. The cation exchange mechanism dominates overall retention for ionized analytes in the silica column (R2 > 0.995), whereas the retention of ionized analytes increases with pH. Impacts of acetonitrile content, buffer ionic strength, and pH, along with their interactions on the retention of ionized analytes in the silica column, were determined using the chemometric approach. Acetonitrile content showed the most significant impact on the retention mechanisms. These findings highlight that a detailed investigation into retention mechanisms provides notable insights into factors influencing analyte retention and separation, promising valuable guidance for future analysis.


Assuntos
Amidas , Amitriptilina , Interações Hidrofóbicas e Hidrofílicas , Dióxido de Silício , Dióxido de Silício/química , Amitriptilina/análise , Amitriptilina/química , Amidas/química , Amidas/análise , Cromatografia Líquida de Alta Pressão , Contaminação de Medicamentos , Cromatografia Líquida/métodos , Estrutura Molecular
10.
J Sep Sci ; 47(9-10): e2400061, 2024 May.
Artigo em Inglês | MEDLINE | ID: mdl-38726749

RESUMO

Determination of proteins from dried matrix spots using MS is an expanding research area. Mainly, the collected dried matrix sample is whole blood from a finger or heal prick, resulting in dried blood spots. However as other matrices such as plasma, serum, urine, and tear fluid also can be collected in this way, the term dried matrix spot is used as an overarching term. In this review, the focus is on advancements in the field made from 2017 up to 2023. In the first part reviews concerning the subject are discussed. After this, advancements made for clinical purposes are highlighted. Both targeted protein analyses, with and without the use of affinity extractions, as well as untargeted, global proteomic approaches are discussed. In the last part, both methodological advancements are being reviewed as well as the possibility to integrate sample preparation steps during the sample handling. The focus, of this so-called smart sampling, is on the incorporation of cell separation, proteolysis, and antibody-based affinity capture.


Assuntos
Teste em Amostras de Sangue Seco , Espectrometria de Massas , Proteínas , Humanos , Cromatografia Líquida , Proteínas/análise , Proteômica/métodos , Manejo de Espécimes , Espectrometria de Massa com Cromatografia Líquida
11.
Se Pu ; 42(5): 445-451, 2024 Apr 08.
Artigo em Chinês | MEDLINE | ID: mdl-38736387

RESUMO

Mycotoxins are toxic secondary metabolites produced by fungal species that can cause acute, subacute, and chronic toxicity in humans and animals. Thus, these toxins pose a significant threat to health and safety. Owing to the lack of effective antimold measures in the agricultural industry, feed ingredients such as corn, peanuts, wheat, barley, millet, nuts, oily feed, forage, and their byproducts are prone to mold and mycotoxin contamination, which can affect animal production, product quality, and safety. Cyclopiazonic acid (CPA), which is mainly biosynthesized from mevalonate, tryptophan, and diacetate units, is a myotoxic secondary metabolite produced by Penicillium and Aspergillus fungi. CPA is widely present as a copollutant with aflatoxins in various crops. Compared with some common mycotoxins such as aflatoxins, fumonisins, ochratoxins, zearalenones, and their metabolites, CPA has not been well investigated. In the United States, a survey showed that 51% of corn and 90% of peanut samples contained CPA, with a maximum level of 2.9 mg/kg. In Europe, CPA was found in Penicillium-contaminated cheeses as high as 4.0 mg/kg. Some studies have shown that CPA can cause irreversible damage to organs such as the liver and spleen in mice. Therefore, the establishment of a rapid and efficient analytical method for CPA is of great significance for the risk assessment of CPA in feeds, the development of standard limits, and the protection of feed product quality and safety. The QuEChERS method, a sample pretreatment method that is fast, simple, cheap, effective, and safe, is widely used in the analysis of pesticide residues in food. In this study, a modified QuEChERS method combined with ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was used to determine CPA levels in feeds. The chromatographic separation and MS detection of CPA as well as the key factors affecting the extraction efficiency of CPA, including the type of extraction solvent, type of inorganic salt, and type and dosage of adsorbent, were optimized in detail. During the optimization of the chromatographic-separation step, the acid and salt concentrations of the mobile phase affected the separation and detection of CPA. During the optimization of the QuEChERS method, the addition of a certain amount of acetic acid improved the extraction efficiency of CPA because of its acidic nature; in addition, GCB and PSA significantly adsorbed CPA from the feed extract. Under optimal conditions, the CPA in the feed sample (1.0 g) was extracted with 2 mL of water and 4 mL of acetonitrile (ACN) containing 0.5% acetic acid. After salting out with 0.4 g of NaCl and 1.6 g of MgSO4, 1 mL of the ACN supernatant was purified by dispersive solid-phase extraction using 150 mg of MgSO4 and 50 mg of C18 and analyzed by UPLC-MS/MS. The sample was separated on a Waters HSS T3 column (100 mm×2.1 mm, 1.8 µm) using 2 mmol/L ammonium acetate aqueous solution with 0.5% formic acid and ACN as the mobile phases and then analyzed by positive electrospray ionization in multiple reaction monitoring mode. CPA exhibited good linearity in the range of 2-200 ng/mL, with a high correlation coefficient (r=0.9995). The limits of detection and quantification of CPA, which were calculated as 3 and 10 times the signal-to-noise ratio, respectively, were 0.6 and 2.0 µg/kg, respectively. The average recoveries in feed samples spiked with 10, 100, and 500 µg/kg CPA ranged from 70.1% to 78.5%, with an intra-day precision of less than 5.8% and an inter-day precision of less than 7.2%, indicating the good accuracy and precision of the proposed method. Finally, the modified QuEChERS-UPLC-MS/MS method was applied to the analysis of CPA in 10 feed samples obtained from Wuhan market. The analysis results indicated that the developed method has good applicability for CPA analysis in feed samples. In summary, an improved QuEChERS method was applied to the extraction and purification of CPA from feeds for the first time; this method provides a suitable analytical method for the risk monitoring, assessment, and standard-limit setting of CPA in feed samples.


Assuntos
Ração Animal , Contaminação de Alimentos , Indóis , Espectrometria de Massas em Tandem , Espectrometria de Massas em Tandem/métodos , Ração Animal/análise , Cromatografia Líquida de Alta Pressão/métodos , Contaminação de Alimentos/análise , Indóis/análise , Micotoxinas/análise
12.
Se Pu ; 42(5): 474-480, 2024 Apr 08.
Artigo em Chinês | MEDLINE | ID: mdl-38736391

RESUMO

A method was established for the simultaneous detection of 12 prohibited veterinary drugs, including ß2-receptor agonists, nitrofuran metabolites, nitroimidazoles, chlorpromazine, and chloramphenicol, in pig urine. The sample was pretreated by enzymolysis, acid hydrolysis/derivatization, and liquid-liquid extraction combined with solid-phase extraction. Detection was performed using ultra high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS). Ammonium acetate solution (0.2 mol/L, 4.5 mL) and ß-glucuronidase/aryl sulfatase (40 µL) were added to the sample, which was subsequently enzymolized at 37 ℃ for 2 h. Then, 1.5 mL of 1.0 mol/L hydrochloric acid solution and 100 µL of 0.1 mol/L o-nitrobenzaldehyde solution were added to the sample. The mixture was incubated at 37 ℃ for 16 h, and the analytes were extracted with 8 mL of ethyl acetate by liquid-liquid extraction. The lower aqueous phase obtained after extraction was extracted and purified using a mixed cation-exchange solid-phase extraction column. The extracts were combined, the extraction solution was blow-dried with nitrogen, and the residue was redissolved for determination. The samples were analyzed under multiple-reaction monitoring mode with both positive and negative electrospray ionization, and quantified using an isotope internal standard method. The correlation coefficients (r) of the 12 compounds were >0.99. The limits of detection (LODs) and quantification (LOQs) of chloramphenicol were 0.05 and 0.1 µg/L, respectively, and the LODs and LOQs of the other compounds were 0.25 and 0.5 µg/L, respectively. The mean recoveries and RSDs at 1, 2, and 10 times the LOQ were 83.6%-115.3% and 2.20%-12.34%, respectively. The proposed method has the advantages of high sensitivity, good stability, and accurate quantification; thus, it is suitable for the simultaneous determination of the 12 prohibited veterinary drug residues in pig urine.


Assuntos
Resíduos de Drogas , Espectrometria de Massas em Tandem , Drogas Veterinárias , Animais , Espectrometria de Massas em Tandem/métodos , Suínos , Cromatografia Líquida de Alta Pressão/métodos , Drogas Veterinárias/urina , Drogas Veterinárias/análise , Resíduos de Drogas/análise , Cloranfenicol/urina , Cloranfenicol/análise
13.
Se Pu ; 42(5): 465-473, 2024 Apr 08.
Artigo em Chinês | MEDLINE | ID: mdl-38736390

RESUMO

A method based on gas chromatography-triple quadrupole mass spectrometry (GC-MS/MS) coupled with one-step QuEChERS technique was developed for the simultaneous determination of 15 N-nitrosamines in air-dried yak meat. The hydration volume, extraction solvent, extracting salt, and cleaning material were optimized according to the characteristics of the N-nitrosamines and sample matrix. The optimized conditions were as follows: 10 mL of purified water for sample hydration, acetonitrile as the extraction solvent for the sample after hydration, 4.0 g of anhydrous MgSO4 and 1.0 g of NaCl as extracting salts, 500 mg of MgSO4+25 mg of C18+50 mg of PSA as cleaning materials. Favorable recoveries of the 15 N-nitrosamines were obtained when the extraction solution was incompletely dried. Thus, the final extract was dried to below 0.5 mL under a mild nitrogen stream and then redissolved to 0.5 mL with acetonitrile. After filtration, 200 µL of the sample was transferred to an autosampler vial for GC-MS/MS analysis. The 15 N-nitrosamines were determined using GC-MS/MS on a DB-HeavyWAX column (30 m×0.25 mm×0.25 µm) with an electron impact ion source in multiple-reaction monitoring (MRM) mode, and quantified using an external standard method. Under the optimized experimental conditions, the results showed that the calibration curves exhibited good linearities for the 15 N-nitrosamines, with correlation coefficients (r2) greater than 0.9990. The limits of detection (LODs) and the limits of quantification (LOQs) ranged from 0.05 to 0.20 µg/kg and from 0.10 to 0.50 µg/kg, respectively. At spiked levels of 1LOQ, 2LOQ, and 10LOQ, the average recoveries were 79.4%-102.1%, 80.6%-109.5%, and 83.0%-110.6%, respectively, and the relative standard deviations were in the range of 0.8%-16.0%. The low matrix effects of the 15 N-nitrosamines indicated the high sensitivity of the proposed method. The method was applied to detect representative commercial air-dried yak meat samples obtained using different processing techniques. Seven N-nitrosamines, including N-nitrosodimethylamine, N-nitrosodiisobutylamine, N-nitrosodibutylamine, N-methyl-N-phenylnitrous amide, N-ethyl-N-nitrosoaniline, N-nitrosopyrrolidine, and N-nitrosodiphenylamine were detected in all samples. The average contents of the seven N-nitrosamines was 0.08-20.18 µg/kg. The detection rates and average contents of the N-nitrosamines in cooked air-dried yak meat samples were higher than those in traditional raw air-dried yak meat samples. Compared with the manual QuEChERS method, the one-step QuEChERS method developed integrated the extraction and clean-up procedures into one single run, and the detection efficiency was considerably improved. The developed method is simple, rapid, highly sensitive, and insusceptible to human errors. Thus, it is useful for the determination of N-nitrosamines in air-dried yak meat and can be extended to the qualitative and quantitative analysis of N-nitrosamines in other meat products. It also provides method support and a data reference for the general determination of N-nitrosamines, which is of great significance for food safety.


Assuntos
Contaminação de Alimentos , Cromatografia Gasosa-Espectrometria de Massas , Carne , Nitrosaminas , Animais , Nitrosaminas/análise , Cromatografia Gasosa-Espectrometria de Massas/métodos , Bovinos , Contaminação de Alimentos/análise , Carne/análise
14.
Se Pu ; 42(5): 481-486, 2024 Apr 08.
Artigo em Chinês | MEDLINE | ID: mdl-38736392

RESUMO

Ibandronate sodium, a third-generation diphosphate drug used worldwide to treat osteoporosis, has the advantages of convenient use, low toxicity, and significant therapeutic effects. However, the residual organic solvents in the synthesis process of sodium ibandronate not only have a negative impact on the efficacy of the drug, but also lead to a decrease in drug stability. Moreover, if the residual amounts of these solvents exceed safety standards, they may pose serious threats to human health. This study successfully established a convenient and efficient method based on headspace-gas chromatography (HS-GC) for the simultaneous determination of five residual solvents (methanol, acetone, benzene, toluene, 1-pentanol) in the raw materials of ibandronate sodium. The results indicated that satisfactory analytical performance can be achieved by using DB-624 capillary column (30 m×0.32 mm×1.8 µm) and a flame ionization detector in conjunction with headspace autosampling and a temperature program. The specific operating conditions included an initial temperature of 40 ℃, with a hold of 2 min, followed by a temperature ramp first to 200 ℃ at a rate of 5 ℃/min and then to 240 ℃ at a rate of 20 ℃/min, with a hold of 5 min. Nitrogen with a flow rate of 1 mL/min and split ratio of 14∶1 was used as the carrier gas. The headspace vial temperature was maintained at 80 ℃, and the sample equilibration time was 20 min. Under the established analytical conditions, good linear relationships were obtained between the mass concentrations of methanol (72-216 µg/mL), acetone (120-360 µg/mL), benzene (0.048-0.144 µg/mL), toluene (21.36-64.08 µg/mL), and 1-pentanol (120-360 µg/mL) and their corresponding peak areas, with correlation coefficients (r) greater than 0.990. The limits of detection for these solvents were 2.88, 0.011, 0.90, 0.24, and 0.024 ng/mL, respectively, with limits of quantification of 11.5, 0.043, 3.6, 0.96, and 0.096 ng/mL, respectively. Furthermore, the recoveries of these solvents ranged from 86.3% to 101.9%, with relative standard deviations (RSDs, n=3) of less than 2.49%. The proposed method is simple, accurate, reliable, and suitable for the rapid and simultaneous determination of five residual solvents in the raw materials of ibandronate sodium. This study has important practical significance in improving drug safety and ensuring public health.


Assuntos
Ácido Ibandrônico , Solventes , Cromatografia Gasosa/métodos , Solventes/química , Ácido Ibandrônico/análise , Difosfonatos/análise , Contaminação de Medicamentos
15.
Front Public Health ; 12: 1375379, 2024.
Artigo em Inglês | MEDLINE | ID: mdl-38737864

RESUMO

Background: Inflammation and liver function are associated with cognitive decline and dementia. Little is known about the serum albumin-to-globulin ratio on cognitive function. Objective: The objective of this study was to investigate the association between albumin-to-globulin ratio and cognitive function among the American older people. Methods: The public data available on the US National Health and Nutrition Examination Survey (NHANES) from 2011 to 2014 was used for this cross-sectional study. Participants aged ≥60 years completed the cognitive function assessments, including word learning and recall modules from the Consortium to Establish a Registry for Alzheimer's Disease (CERAD), the animal fluency (AF) test, and the digit symbol substitution test (DSST). A composite cognition score was calculated to evaluate global cognition. The univariate and multivariate linear regression analysis, curve fitting, a threshold effect, along with a subgroup analysis and interaction tests were conducted. Results: Serum albumin-to-globulin ratio (per 0.1 unit) was positively associated DSST score (ß = 0.36, 95% CI: 0.21, 0.51), AF score (ß = 0.1, 95% CI: 0.04, 0.16) and global cognition score (ß = 0.05, 95% CI: 0.02, 0.07), after being fully adjusted, while albumin-to-globulin ratio was not related to CERAD score (ß = 0.05, 95% CI: -0.02, 0.12). A non-linear was observed in the dose-response relationship between albumin-to-globulin ratio and global cognition (P for non-linearity < 0.001). The subgroup analysis was overall stable, yet the interaction test was significant for age on global cognition (P for interaction = 0.036). Conclusion: The findings of this cross-sectional study suggested a positive and non-linear association between albumin-to-globulin ratio and cognitive function in the American older people. Maintaining albumin-to-globulin ratio with an appropriate range may be one of the therapeutic strategies to limit the progression of cognitive decline for the older people.


Assuntos
Cognição , Inquéritos Nutricionais , Albumina Sérica , Humanos , Estudos Transversais , Masculino , Feminino , Idoso , Cognição/fisiologia , Estados Unidos , Pessoa de Meia-Idade , Albumina Sérica/análise , Disfunção Cognitiva/sangue , Idoso de 80 Anos ou mais , Soroglobulinas/análise , Globulinas/análise
16.
Endocrinol Diabetes Metab ; 7(3): e00484, 2024 May.
Artigo em Inglês | MEDLINE | ID: mdl-38739122

RESUMO

OBJECTIVE: This study investigates the metabolic differences between normal, prediabetic and diabetic patients with good and poor glycaemic control (GGC and PGC). DESIGN: In this study, 1102 individuals were included, and 50 metabolites were analysed using tandem mass spectrometry. The diabetes diagnosis and treatment standards of the American Diabetes Association (ADA) were used to classify patients. METHODS: The nearest neighbour method was used to match controls and cases in each group on the basis of age, sex and BMI. Factor analysis was used to reduce the number of variables and find influential underlying factors. Finally, Pearson's correlation coefficient was used to check the correlation between both glucose and HbAc1 as independent factors with binary classes. RESULTS: Amino acids such as glycine, serine and proline, and acylcarnitines (AcylCs) such as C16 and C18 showed significant differences between the prediabetes and normal groups. Additionally, several metabolites, including C0, C5, C8 and C16, showed significant differences between the diabetes and normal groups. Moreover, the study found that several metabolites significantly differed between the GGC and PGC diabetes groups, such as C2, C6, C10, C16 and C18. The correlation analysis revealed that glucose and HbA1c levels significantly correlated with several metabolites, including glycine, serine and C16, in both the prediabetes and diabetes groups. Additionally, the correlation analysis showed that HbA1c significantly correlated with several metabolites, such as C2, C5 and C18, in the controlled and uncontrolled diabetes groups. CONCLUSIONS: These findings could help identify new biomarkers or underlying markers for the early detection and management of diabetes.


Assuntos
Carnitina/análogos & derivados , Metabolômica , Estado Pré-Diabético , Espectrometria de Massas em Tandem , Humanos , Estado Pré-Diabético/diagnóstico , Estado Pré-Diabético/metabolismo , Metabolômica/métodos , Masculino , Espectrometria de Massas em Tandem/métodos , Feminino , Pessoa de Meia-Idade , Adulto , Hemoglobinas Glicadas/metabolismo , Hemoglobinas Glicadas/análise , Glicemia/metabolismo , Diabetes Mellitus/metabolismo , Diabetes Mellitus/sangue , Diabetes Mellitus/diagnóstico , Idoso , Biomarcadores/sangue , Diabetes Mellitus Tipo 2/metabolismo , Diabetes Mellitus Tipo 2/diagnóstico , Metaboloma , Controle Glicêmico
17.
PLoS One ; 19(5): e0301605, 2024.
Artigo em Inglês | MEDLINE | ID: mdl-38739592

RESUMO

Oxygen minimum zones (OMZ) represent ~8% of the ocean, with the Pacific as the largest and top expanding area. These regions influence marine ecosystems, promoting anaerobic microbial communities. Nevertheless, only a fraction of microbial diversity has been studied, with fungi being the less explored component. So, herein we analyzed fungal diversity patterns in surface and subsurface sediments along a bathymetric transect using metabarcoding of the ITS1 region in the OMZ of the Mexican Pacific off Mazatlán. We identified 353 amplicon sequence variants (ASV), within the Ascomycota, Basidiomycota, and Rozellomycota. Spatial patterns evidenced higher alpha diversity in nearshore and subsurface subsamples, probably due to temporal fluctuations in organic matter inputs. Small-scale heterogeneity characterized the community with the majority of ASV (269 ASV) occurring in a single subsample, hinting at the influence of local biogeochemical conditions. This baseline data evidenced a remarkable fungal diversity presenting high variation along a bathymetric and vertical transects.


Assuntos
Biodiversidade , Código de Barras de DNA Taxonômico , Fungos , Sedimentos Geológicos , Oxigênio , Sedimentos Geológicos/microbiologia , Oxigênio/metabolismo , Oxigênio/análise , Fungos/genética , Fungos/classificação , Fungos/isolamento & purificação , Oceano Pacífico , Filogenia
18.
PLoS One ; 19(5): e0300573, 2024.
Artigo em Inglês | MEDLINE | ID: mdl-38739594

RESUMO

The intercropping system is a promising approach to augmenting the soil nutrient status and promoting sustainable crop production. However, it is not known whether intercropping improves the soil phosphorus (P) status in alluvial soils with low P under subtropical climates. Over two growing seasons--2019-2020 and 2020-2021--two experimental fields were employed to explore the effect of durum wheat (Dw) and chickpea (Cp) cropping systems on the soil available P. A randomized complete block design was used in this experiment, with three blocks each divided into three plots. Each plot was used for one of the following three treatments with three replications: Dw monocrop (Dw-MC), Cp monocrop (Cp-MC), and Dw + Cp intercrop (CpDw-InC), with bulk soil (BS) used as a control. A reduction in the rhizosphere soil pH (-0.44 and -0.11 unit) was observed in the (Cp-MC) and (CpDw-InC) treatments over BS, occurring concomitantly with a significant increase in available P in the rhizosphere soil of around 28.45% for CpDw-InC and 24.9% for Cp-MC over BS. Conversely, the rhizosphere soil pH was significantly higher (+0.12 units) in the Dw-MC treatments. In addition, intercropping enhanced the soil microbial biomass P, with strong positive correlations observed between the biomass P and available P in the Cp-MC treatment, whereas this correlation was negative in the CpDw-InC and Dw-MC treatments. These findings suggested that Cp intercropped with Dw could be a viable approach in enhancing the available P through improved pH variation and biomass P when cultivated on alluvial soil under a subtropical climate.


Assuntos
Biomassa , Cicer , Fósforo , Solo , Triticum , Fósforo/análise , Fósforo/metabolismo , Triticum/crescimento & desenvolvimento , Triticum/metabolismo , Solo/química , Cicer/crescimento & desenvolvimento , Cicer/metabolismo , Agricultura/métodos , Rizosfera , Clima Tropical , Produtos Agrícolas/crescimento & desenvolvimento , Produção Agrícola/métodos , Concentração de Íons de Hidrogênio , Clima
19.
PLoS One ; 19(5): e0302883, 2024.
Artigo em Inglês | MEDLINE | ID: mdl-38739605

RESUMO

Anemia is defined as a low hemoglobin (Hb) concentration and is highly prevalent worldwide. We report on the performance of a smartphone application (app) that records images in RAW format of the palpebral conjunctivae and estimates Hb concentration by relying upon computation of the tissue surface high hue ratio. Images of bilateral conjunctivae were obtained prospectively from a convenience sample of 435 Emergency Department patients using a dedicated smartphone. A previous computer-based and validated derivation data set associating estimated conjunctival Hb (HBc) and the actual laboratory-determined Hb (HBl) was used in deriving Hb estimations using a self-contained mobile app. Accuracy of HBc was 75.4% (95% CI 71.3, 79.4%) for all categories of anemia, and Bland-Altman plot analysis showed a bias of 0.10 and limits of agreement (LOA) of (-4.73, 4.93 g/dL). Analysis of HBc estimation accuracy around different anemia thresholds showed that AUC was maximized at transfusion thresholds of 7 and 9 g/dL which showed AUC values of 0.92 and 0.90 respectively. We found that the app is sufficiently accurate for detecting severe anemia and shows promise as a population-sourced screening platform or as a non-invasive point-of-care anemia classifier.


Assuntos
Anemia , Túnica Conjuntiva , Hemoglobinas , Smartphone , Humanos , Anemia/diagnóstico , Túnica Conjuntiva/irrigação sanguínea , Túnica Conjuntiva/patologia , Feminino , Masculino , Hemoglobinas/análise , Pessoa de Meia-Idade , Adulto , Aplicativos Móveis , Idoso , Estudos Prospectivos , Processamento de Imagem Assistida por Computador/métodos , Idoso de 80 Anos ou mais
20.
PLoS One ; 19(5): e0303101, 2024.
Artigo em Inglês | MEDLINE | ID: mdl-38739642

RESUMO

This research study aims to understand the application of Artificial Neural Networks (ANNs) to forecast the Self-Compacting Recycled Coarse Aggregate Concrete (SCRCAC) compressive strength. From different literature, 602 available data sets from SCRCAC mix designs are collected, and the data are rearranged, reconstructed, trained and tested for the ANN model development. The models were established using seven input variables: the mass of cementitious content, water, natural coarse aggregate content, natural fine aggregate content, recycled coarse aggregate content, chemical admixture and mineral admixture used in the SCRCAC mix designs. Two normalization techniques are used for data normalization to visualize the data distribution. For each normalization technique, three transfer functions are used for modelling. In total, six different types of models were run in MATLAB and used to estimate the 28th day SCRCAC compressive strength. Normalization technique 2 performs better than 1 and TANSING is the best transfer function. The best k-fold cross-validation fold is k = 7. The coefficient of determination for predicted and actual compressive strength is 0.78 for training and 0.86 for testing. The impact of the number of neurons and layers on the model was performed. Inputs from standards are used to forecast the 28th day compressive strength. Apart from ANN, Machine Learning (ML) techniques like random forest, extra trees, extreme boosting and light gradient boosting techniques are adopted to predict the 28th day compressive strength of SCRCAC. Compared to ML, ANN prediction shows better results in terms of sensitive analysis. The study also extended to determine 28th day compressive strength from experimental work and compared it with 28th day compressive strength from ANN best model. Standard and ANN mix designs have similar fresh and hardened properties. The average compressive strength from ANN model and experimental results are 39.067 and 38.36 MPa, respectively with correlation coefficient is 1. It appears that ANN can validly predict the compressive strength of concrete.


Assuntos
Força Compressiva , Materiais de Construção , Aprendizado de Máquina , Redes Neurais de Computação , Materiais de Construção/análise , Reciclagem
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