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1.
Anal Chim Acta ; 1191: 339286, 2022 Jan 25.
Artigo em Inglês | MEDLINE | ID: mdl-35033253

RESUMO

Inositol phosphates belong to a family of structurally diverse signaling molecules playing crucial role in Ca2+ release from intracellular storage vesicles. There are many possibilities of phosphorylation, including their degree and position. Inositol (1,4,5) trisphosphate has been well recognized as the most important second messenger among this family. It remains a challenge to analyse the entire inositol phosphate metabolite family due to its structural complexity, high polarity, and high phosphate density. In this study, we have established an improved UHPLC-ESI-MS/MS method based on a differential isotope labelling methylation strategy. An SPE extraction kit composed of TiO2 and PTFE filter was employed for sample preparation which provided good extraction performance. Samples were methylated (light label) to neutralize the phosphate groups and give better performance in liquid chromatography. Regioisomers and inositol phosphates differing in their number of phosphate residues were successfully separated after optimization on a core-shell cholesterylether-bonded RP-type column (Cosmocore 2.6Cholester) using methanol as organic modifier. Triple quadrupole MS detection was based on selected reaction monitoring (SRM) acquisition with characteristic fragments. Stable isotope labeling methylation was performed to generate internal standards (heavy label). Limits of quantification from 0.32 to 0.89 pmol on column was achieved. This method was validated to be suitable for inositol phosphate profiling in biological samples. After application in cultured HeLa cells, NIST SRM1950 plasma, and human platelets, distinct inositol profiles were obtained. This newly established method exhibited improved analytical performance, holding the potential to advance the understanding of inositol phosphate signaling.


Assuntos
Extração em Fase Sólida , Espectrometria de Massas em Tandem , Cromatografia Líquida de Alta Pressão , Cromatografia Líquida , Células HeLa , Humanos , Fosfatos de Inositol , Marcação por Isótopo , Metilação , Fosfatos
2.
Food Chem ; 374: 131778, 2022 Apr 16.
Artigo em Inglês | MEDLINE | ID: mdl-35021580

RESUMO

Core-shell structured magnetic covalent-organic frameworks (Fe3O4@TaTp) were facilely synthesized based on one-step functionalization at room temperature and applied for magnetic solid-phase extraction of okadaic acid from seawater and shellfish prior to LC-MS/MS detection. Parameters, including adsorbent amount, extraction time, desorption solution, and desorption time which could affect the extraction efficiency, were respectively investigated. The developed methods demonstrated good linearity (R2 > 0.99), acceptable accuracy and good precision (<15%), and low limit of detection (0.5 pg·mL-1 for seawater and 0.04 µg·kg-1 for shellfish). The amount of the material used (1 mg for seawater and 5 mg for shellfish) and the time required (4 min for seawater and 15 min for shellfish) for extracting analyte from 5 mL of seawater and 2 g of shellfish are both greatly shortened compared with the previous reports. In addition, we successfully applied this method to real sample analysis.


Assuntos
Estruturas Metalorgânicas , Adsorção , Cromatografia Líquida , Limite de Detecção , Fenômenos Magnéticos , Ácido Okadáico/análise , Água do Mar , Frutos do Mar/análise , Extração em Fase Sólida , Espectrometria de Massas em Tandem
3.
Food Chem ; 376: 131835, 2022 May 15.
Artigo em Inglês | MEDLINE | ID: mdl-34980530

RESUMO

To reduce matrix interference and realize simultaneous detection of multiple homologous compounds (trimethoprim (TMP), diaveridine (DVD), ormetoprim (OMP), baquiloprim (BQP), and aditoprim (ADP) in pig, cattle, chicken, and fish muscles), an immunomagnetic bead (IMB)-based sample purification pretreatment with HPLC-UV was developed. A broad-spectrum monoclonal antibody (mAb, named 14C6) was prepared and conjugated with carboxylic-acid-functionalized magnetic nanoparticles using the active ester method to obtain IMBs for sample purification. The extraction solvent was optimized based on the extraction efficiency. Good linearity was observed for all the five analytes (10-200 µg/kg) with the LOD and LOQ of 5 and 10 µg/kg, respectively. The mean recoveries ranged from 62.5% to 76.9%, while the coefficient of variation was <12.2%. The IMB method afforded greater sample purification and enrichment than those achieved with the SPE column-based conventional method. Hence, the IMB-based sample purification is a useful tool to determine 2,4-diaminopyrimidine residues in edible animal tissues.


Assuntos
Contaminação de Alimentos/análise , Carne/análise , Pirimidinas/análise , Extração em Fase Sólida , Espectrometria de Massas em Tandem , Animais , Bovinos , Galinhas , Cromatografia Líquida de Alta Pressão , Peixes , Suínos
4.
Environ Int ; 158: 106996, 2022 01.
Artigo em Inglês | MEDLINE | ID: mdl-34991256

RESUMO

A multi-specimen, multi-mycotoxin approach involving ultra-sensitive LC-MS/MS analysis of breast milk, complementary food and urine was applied to examine mycotoxin co-exposure in 65 infants, aged 1-18 months, in Ogun state, Nigeria. Aflatoxin M1 was detected in breast milk (4/22 (18%)), while six other classes of mycotoxins were quantified; including dihydrocitrinone (6/22 (27%); range: 14.0-59.7 ng/L) and sterigmatocystin (1/22 (5%); 1.2 ng/L) detected for the first time. Seven distinct classes of mycotoxins including aflatoxins (9/42 (21%); range: 1.0-16.2 µg/kg) and fumonisins (12/42 (29%); range: 7.9-194 µg/kg) contaminated complementary food. Mycotoxins covering seven distinct classes with diverse structures and modes of action were detected in 64/65 (99%) of the urine samples, demonstrating ubiquitous exposure. Two aflatoxin metabolites (AFM1 and AFQ1) and FB1 were detected in 6/65 (9%), 44/65 (68%) and 17/65 (26%) of urine samples, respectively. Mixtures of mycotoxin classes were common, including 22/22 (100%), 14/42 (33%) and 56/65 (86%) samples having 2-6, 2-4, or 2-6 mycotoxins present, for breast milk, complementary food and urine, respectively. Aflatoxin and/or fumonisin was detected in 4/22 (18%), 12/42 (29%) and 46/65 (71%) for breast milk, complimentary foods and urine, respectively. Furthermore, the detection frequency, median concentrations and occurrence of mixtures were typically greater in urine of non-exclusively breastfed compared to exclusively breastfed infants. The study provides novel insights into mycotoxin co-exposures in early-life. Albeit a small sample set, it highlights transition to higher levels of infant mycotoxin exposure as complementary foods are introduced, providing impetus to mitigate during this critical early-life period and encourage breastfeeding.


Assuntos
Citrinina , Micotoxinas , Monitoramento Biológico , Biomarcadores , Aleitamento Materno , Criança , Cromatografia Líquida , Feminino , Contaminação de Alimentos/análise , Humanos , Lactente , Leite Humano/química , Nigéria , Espectrometria de Massas em Tandem
5.
Microb Cell Fact ; 21(1): 4, 2022 Jan 04.
Artigo em Inglês | MEDLINE | ID: mdl-34983528

RESUMO

Given a serious threat of multidrug-resistant bacterial pathogens to global healthcare, there is an urgent need to find effective antibacterial compounds to treat drug-resistant bacterial infections. In our previous studies, Bacillus velezensis CB6 with broad-spectrum antibacterial activity was obtained from the soil of Changbaishan, China. In this study, with methicillin-resistant Staphylococcus aureus as an indicator bacterium, an antibacterial protein was purified by ammonium sulfate precipitation, Sephadex G-75 column, QAE-Sephadex A 25 column and RP-HPLC, which demonstrated a molecular weight of 31.405 kDa by SDS-PAGE. LC-MS/MS analysis indicated that the compound was an antibacterial protein CB6-C, which had 88.5% identity with chitosanase (Csn) produced by Bacillus subtilis 168. An antibacterial protein CB6-C showed an effective antimicrobial activity against gram-positive bacteria (in particular, the MIC for MRSA was 16 µg/mL), low toxicity, thermostability, stability in different organic reagents and pH values, and an additive effect with conventionally used antibiotics. Mechanistic studies showed that an antibacterial protein CB6-C exerted anti-MRSA activity through destruction of lipoteichoic acid (LTA) on the cell wall. In addition, an antibacterial protein CB6-C was efficient in preventing MRSA infections in in vivo models. In conclusion, this protein CB6-C is a newly discovered antibacterial protein and has the potential to become an effective antibacterial agent due to its high therapeutic index, safety, nontoxicity and great stability.


Assuntos
Antibacterianos/farmacologia , Proteínas de Bactérias/farmacologia , Staphylococcus aureus Resistente à Meticilina/efeitos dos fármacos , Animais , Antibacterianos/uso terapêutico , Bacillus/química , Bacillus/enzimologia , Proteínas de Bactérias/química , Proteínas de Bactérias/isolamento & purificação , China , Cromatografia Líquida , Farmacorresistência Bacteriana Múltipla , Feminino , Camundongos , Camundongos Endogâmicos BALB C , Testes de Sensibilidade Microbiana , Infecções Estafilocócicas/tratamento farmacológico , Espectrometria de Massas em Tandem
6.
Se Pu ; 40(1): 28-40, 2022 Jan.
Artigo em Chinês | MEDLINE | ID: mdl-34985213

RESUMO

Given the wide variety of fentanyl analogs, the test for this entire group tends to be crucial and particularly difficult since all fentanyl-like substances are listed as controlled substances in China. This study meticulously analyzed the fragmentation pathways and mechanisms of 29 fentanyl analogs and summarized the fragmentation pathways and features for the entire group of fentanyl analogs, thus providing a reference for related screening tests. Fentanyl, thiofentanyl, and sufentanil were selected as the representative compounds in this study, and the fragmentation mechanism of their fragment ions was interpreted. The general fragmentation rules for fentanyl analogs were summarized as well. The fragment ions of the three compounds formed by induced cleavage (i) came with high abundance ratios, such as fragment ions of m/z 188, 105, 194, 111, and 238, while the induced cleavage was due to the amide and piperidinyl groups. Moreover, the induction ability of amide group was significantly stronger than that of the piperidinyl group, and induced cleavage was the main fragmentation pathway for most of the fentanyl analogs. Furthermore, the fragment ions with m/z 281 and 287 for fentanyl and thiofentanyl were formed by loss of the propionyl group after single H rearrangement (rH). The fragment ions with m/z 216, 146, and 132 for fentanyl and thiofentanyl were formed by double H rearrangement (r2H). Although their abundance ratios were not high, they still had specificity and regularity. Elimination reaction (re) was also a very common fragmentation pathway for these compounds, leading to fragment ions with m/z 134 and 140. Phenylethyl substituents were more prone to the elimination reaction with a higher abundance ratio than thiophenethyl substituents. Compounds such as sufentanil with methoxy substituents at the piperidinyl para-position could produce a large number of fragment ions, which were more susceptible to the rH pathway and loss of methanol neutral molecules, leading to the formation of ions with m/z 355. Similarly, compounds such as remifentanil bearing a methyl formate substituent at the piperidine para-position also produced numerous fragment ions, which were more prone to the rH pathway to lose methyl formate or methanol neutral molecules and furnish fragment ions with m/z 317 or 345. Compounds containing hydroxyl substituents, such as ß-hydroxyfentanyl and ß-hydroxythiofentanyl, produce significant dehydration ions and formed fragment ions with m/z 335 (ß-hydroxyfentanyl) and m/z 341 (ß-hydroxythiofentanyl). A method based on liquid chromatography-quadrupole time-of-flight mass spectrometry (LC-QTOF-MS) for the qualitative and quantitative determination of the 29 fentanyl analogs was developed. Drugs and white powder samples were extracted by acetonitrile, as well as protein and milk beverage samples. Sugar-containing solids or powders, drinking water, fruit and vegetable drinks, health drinks, tea drinks, and alcohol samples were extracted by 10% acetonitrile aqueous solution. Following vortexing, centrifugation, and membrane separation, the target compounds were separated on a Kinetex C18 column (100 mm×2.1 mm, 2.6 µm) with gradient elution at a flow rate of 0.4 mL/min. The mobile phases were composed of acetonitrile and 0.08% formic acid aqueous solution. The target compounds were quantified by LC-QTOF-MS using an external standard method in positive ion mode. The 29 fentanyl analogs showed good linear relationships in the range of 1-20 µg/L, and the correlation coefficients were greater than 0.995. The limits of detection (LODs) and limits of quantification (LOQs) were 0.01 mg/kg and 0.05, respectively. The average recoveries were 85.2%-112.9% for hypoglycemic drugs, Lulu drinks, glucose powder, Zhenlu health drink and chocolate, with RSDs of 1.9%-19.8% (n=6). This method is rapid, simple, time-saving, highly sensitivity and stable, and it is applicable to a wide variety of samples. Hence, it is suitable for the identification, confirmation, and quantitative detection of the 29 fentanyl analogs in drugs, solids or powders containing sugar, beverages, drinking water, wine samples, etc.


Assuntos
Fentanila , Espectrometria de Massas em Tandem , Cromatografia Líquida de Alta Pressão , Cromatografia Líquida , Verduras
7.
Se Pu ; 40(1): 41-47, 2022 Jan.
Artigo em Chinês | MEDLINE | ID: mdl-34985214

RESUMO

Chlorpropham is a plant growth regulator and a herbicide. It is commonly used in the post-harvest treatment of potato to inhibit germination. It can also be used for flower thinning and fruit thinning of fruit trees, and for controlling annual gramineous weeds and a few broad-leaved weeds. Improper or excessive use of chlorpropham in crop cultivation will affect the safety of animal-derived food and impair human health through the food chain and water cycle. Therefore, accurate quantification of chlorpropham is imperative for risk assessment and mitigating risks to food safety. A method based on solid phase extraction and ultra-high performance liquid chromatography-tandem mass spectrometry (SPE-UHPLC-MS/MS) was established for the determination of chlorpropham in animal-derived food. First, the pretreatment conditions were optimized. To purify the samples and remove impurities, SPE column cartridges with different packing materials such as PXC, PXA, Florisil, and PLS were investigated. Based on the retention of chlorpropham, the ProElut PLS SPE column was selected as the pretreatment purification column. The washing solution and eluents were then optimized. When water was used as the washing solution, chlorpropham remained adsorbed on the SPE column and was not eluted along with other water-soluble substances. When the proportion of acetonitrile exceeded 40%, chlorpropham adsorbed on the filler of the SPE column could be gradually washed down. Acetonitrile-water solution(30∶70, v/v) was used for washing the SPE column. The elution ability of seven eluents for chlorpropham on the SPE column was then investigated. Among them, pure methanol, pure acetonitrile, and 1% (v/v) formic acid-methanol showed better elution effect. Considering that acetonitrile was used in the sample extraction, it was chosen as the mobile phase eluent. Subsequently, the chromatographic conditions and MS parameters were optimized. By examining the ionization cracking of chlorpropham, the quasimolecular ions and corresponding fragmentations in the chlorpropham primary MS were determined. The separation effect of three C18 columns was investigated. Based on the retention ability and peak effect of chlorpropham on the column, the Agilent ZORBAX SB-C18 (150 mm×2.1 mm, 5 µm) column was used for chlorpropham separation. The response of chlorpropham in the positive and negative ionization modes was investigated and optimized. The results showed that the response was better in the positive ion mode than that in the negative ion mode. After optimizing the chromatographic conditions and MS parameters, the sensitivity of the method was improved. Finally, the analytes were separated on the Agilent ZORBAX SB-C18 (150 mm×2.1 mm, 5 µm) under a gradient elution program using acetonitrile and 0.2% (v/v) formic acid aqueous solution as the mobile phases. The analytes were detected in the multiple reaction monitoring (MRM) mode under positive electrospray ionization (ESI+) conditions. The standard curve solutions were prepared using the matrix solution and quantified by the external standard method. The results showed a good linear relationship in the range of 0.5-100.0 µg/L, with correlation coefficients (r2) greater than 0.9929. The limit of quantification (LOQ) of this method was 3 µg/kg (S/N ≥ 10). At three spiked levels (0.003, 0.006, and 0.060 mg/kg) in 13 animal-derived foods (pork, milk, beef, chicken, duck, egg, chicken gizzard, duck egg, pork kidney, pork liver, beef liver, mutton, duck gizzard), the average recoveries were in the range of 74.9% to 97.6%, and the RSDs were in the range of 2.9% to 9.5% (n=6). Sixty batches of animal-derived food available on the market were analyzed by the developed method, and chlorpropham was not detected in any of these foods. The developed method is rapid, sensitive, and accurate, and it is suitable for the qualitative and quantitative detection of chlorpropham in a variety of animal-derived foods.


Assuntos
Clorprofam , Espectrometria de Massas em Tandem , Animais , Bovinos , Cromatografia Líquida de Alta Pressão , Humanos , Leite , Extração em Fase Sólida
8.
Se Pu ; 40(1): 57-65, 2022 Jan.
Artigo em Chinês | MEDLINE | ID: mdl-34985216

RESUMO

Chromatography combined with mass spectrometry is the most commonly used detection technology, and it offers the advantages of high sensitivity and high selectivity. However, the contents of bisphenols (BPs) in water samples are at the ng/L level. Even if the BPs contents are determined by mass spectrometry, the samples must be pretreated and enriched. A quick, easy, inexpensive, effective, rugged, and safe technique (QuEChERS) can offer advantages such as cost effectiveness and time efficiency. The application of QuEChERS is currently extended to the analysis of contaminants in food and water samples. In this work, QuEChERS coupled with ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was proposed for the determination of eight BPs in surface water. Method optimization was carried out in terms of process efficiency (PE), which included the matrix effect (ME) and extraction recovery (RE). First, the water samples were extracted with 10 mL ethyl acetate and cleaned with 50 mg primary secondary amine (PSA) and 50 mg graphitized carbon black (GCB). Then, the organic layer was collected and evaporated to dryness under nitrogen flow (40 ℃). Finally, the extracts were redissolved in 0.5 mL of a methanol-water (1∶1, v/v) mixture and subjected to UPLC-MS/MS analysis. Chromatographic separation was accomplished on a Waters ACQUITY UPLC BEH C18 column (100 mm×2.1 mm, 1.7 µm) with gradient elution. Methanol and 0.1 mmol/L ammonium bicarbonate aqueous solution were used as the mobile phases. The eight BPs were analyzed by MS/MS with negative electrospray ionization (ESI-) and in the multiple reaction monitoring (MRM) mode. The matrix matching external standard method was used for quantitative determination. The eight compounds could be analyzed within 8 min. Under the optimized conditions, the calibration curves showed good linearities for the eight BPs, and the coefficients of determination (R2) were greater than 0.9990. The limits of detection (LODs, S/N=3) and limits of quantification (LOQs, S/N=10) were in the ranges of 0.1-2.3 ng/L and 0.3-6.1 ng/L, respectively. The average recoveries of the eight BPs in river water samples were 78.8%-116.6%, and the corresponding relative standard deviations (RSDs) were 1.8%-9.0% (n=6). This method was applied to the analysis of BPs pollution in Guangyuan section of Jialing river and its tributaries, and widespread pollution was confirmed. The detection rate of BPA was 100% with a content of 6.15-90.03 ng/L, and the detection rate of BPS was 91%, with the contents being in the range not detected (nd) to 4.63 ng/L. The method established in this study allowed for the rapid enrichment and purification of the eight BPs in water. With its advantages of simplicity, rapidness, high sensitivity, and low cost, the method can be used for the rapid determination of trace BPs in surface water such as lake water and river water.


Assuntos
Extração em Fase Sólida , Espectrometria de Massas em Tandem , Cromatografia Líquida de Alta Pressão , Cromatografia Líquida , Água
9.
Food Chem ; 374: 131761, 2022 Apr 16.
Artigo em Inglês | MEDLINE | ID: mdl-34896946

RESUMO

A rapid, selective, and sensitive method was developed for the detection of carbendazim and thiabendazole in edible vegetable oil. Two benzimidazole analytes were pre-concentrated by magnetic solid phase extraction (MSPE) using flowerlike Ni-NiO composite as sorbents and followed by LC-MS/MS analysis. The flowerlike Ni-NiO composite sorbent displayed a high affinity towards benzimidazole analytes due to the reversible coordination interaction between the Ni(Ⅱ) ion and the electron-donating imidazole group. In comparison to the previous methods, this procedure is less time-consuming and simpler during sample preparation. The parameters affecting the extraction efficiency were optimized in detail. The method was validated according to SANTE/12682/2019. The limits of detection were in the range of 0.001-0.003 mg•kg-1. The recoveries ranged from 89.3% to 110.7% with inter-day and inter-day precision less than 10.9%. The results indicate that flowerlike Ni-NiO composite might be a promising alternative for MSPE of benzimidazole compounds in foods.


Assuntos
Tiabendazol , Verduras , Benzimidazóis/análise , Carbamatos , Cromatografia Líquida de Alta Pressão , Cromatografia Líquida , Fenômenos Magnéticos , Óleos Vegetais , Extração em Fase Sólida , Espectrometria de Massas em Tandem
10.
Food Chem ; 374: 131776, 2022 Apr 16.
Artigo em Inglês | MEDLINE | ID: mdl-34896957

RESUMO

Reducing salt intake, as one of the most cost-effective approaches, is congruent with improved population health. Grass carp skin collagen was subjected to enzymatic hydrolysis and ultrafiltration, followed by glucosamine-induced Maillard reaction to prepare Maillard-reacted peptides. Their color, free amino acid and peptide size distribution were analyzed, while UV and fluorescence spectroscopy were utilized to characterize the progress of Maillard reaction. The salt taste-enhancing effect of Maillard-reacted peptides was investigated via sensory analysis and electronic tongue. LC-MS/MS was employed to analyze the glycation sites of Maillard-reacted peptides. The results indicated that the degree of Maillard reaction was relatively low, and thermal degradation and crosslinking simultaneously occurred. Maillard-reacted peptides exhibited a significant salt taste-enhancing effect, which may be attributed to the glucosamine-induced glycation confirmed by LC-MS/MS analysis. The current study provides a theoretical basis for preparation of salt taste-enhancing peptides and their future application to reduce salt content of formulated foods.


Assuntos
Glucosamina , Paladar , Cromatografia Líquida , Produtos Finais de Glicação Avançada , Reação de Maillard , Peptídeos , Espectrometria de Massas em Tandem
11.
Food Chem ; 374: 131796, 2022 Apr 16.
Artigo em Inglês | MEDLINE | ID: mdl-34906807

RESUMO

Six grades of Huangshan Maofeng (HSMF) green tea were studied by LC-MS based metabolomics combined with sensory evaluation on bitterness, astringency and sweet aftertaste. Although there was no significant correlation (p > 0.05) between tea grades and the contents of total polyphenols and flavonoids, non-targeted metabolomics revealed that all grades of tea could be classified into two groups, group 1 (T1, T2) and group 2 (T3, 1, 2, 3). The main marker compounds responsible for distinguishing the two groups were procyanidins, flavonoid glycosides, and four hydrolysable tannins, including monogalloyl glucose, digalloyl glucose, trigalloyl glucose and galloyl-hexahydroxydiphenoyl-glucose. The Pearson correlation coefficients of these hydrolysable tannins with HSMF green tea grades were between 0.82 and 0.95. Furthermore, their Pearson correlation coefficients regarding sweet aftertaste were in the range of 0.73-0.83. This study suggested combination of metabolomics and sensory evaluation could provide an insight in searching for more potential taste-active components.


Assuntos
Espectrometria de Massas em Tandem , Chá , Cromatografia Líquida , Metabolômica , Polifenóis/análise
12.
J Pharm Biomed Anal ; 209: 114526, 2022 Feb 05.
Artigo em Inglês | MEDLINE | ID: mdl-34915323

RESUMO

Pogostemon cablin Benth (PCB) is a well-known traditional Chinese medicine that has been used for treatment of many ailments for several centuries. In presently, the chemical profiling and quality control study of PCB has mainly concentrated on the volatile fractions. However, the non-volatile chemical profile of PCB was still unclear. In this study, 73 non-volatile constituents (i.e., 33 flavonoids, 21 organic acids, 9 phenylpropanoids, 4 sesquiterpenes, 3 alkaloids, and 3 other types of compounds) were identified and characterized in PCB using high performance liquid chromatography coupled with quadruple time-of-flight tandem mass spectrometry (HPLC-Q-TOF-MS). Meanwhile, to assess PCB samples, an established HPLC-Q-TOF-MS fingerprint was combined with multivariate statistical analysis that included similarity analysis (SA), hierarchical cluster analysis (HCA), principal component analysis (PCA), and orthogonal partial least squares-discriminant analysis (OPLS-DA). The PCB samples could be classified into two groups (herbal decoction pieces and processed medicinal materials), and acteoside, isoacteoside, 4',6-Dihydroxy-5,7-dimethoxyflavone, pachypodol and pogostone were screened as the potential chemical markers that attributed classification. In addition, nine representative components (pachypodol, vicenin-2, apigenin, rhamnocitrin, acteoside, isoacteoside, chlorogenic acid, azelaic acid and pogostone) in PCB were simultaneously determined by using an ultra-high-performance liquid chromatography coupled with triple quadrupole tandem mass spectrometry (UPLC-QQQ-MS/MS). This study is the first to describe the chemical profile of PCB using liquid chromatography tandem mass spectrometry, which would improve our understanding of the substance basis of PCB and is helpful to the PCB further quality evaluation.


Assuntos
Medicamentos de Ervas Chinesas , Pogostemon , Cromatografia Líquida de Alta Pressão , Medicamentos de Ervas Chinesas/análise , Pogostemon/química , Espectrometria de Massas em Tandem
13.
Food Chem ; 374: 131793, 2022 Apr 16.
Artigo em Inglês | MEDLINE | ID: mdl-34915370

RESUMO

The analysis of free fatty acids (FFAs) in edible oils, especially their fine structure, can provide information for nutritional value evaluation and authentication. Here, a strategy based on epoxidation reaction by mCPBA combined with tandem MS was developed to identify and relatively quantify FFAs, including CC location isomers, which can rapidly distinguish different edible oils. Notably, low-abundant FFAs can be detected directly in the presence of high-abundant triacylglycerol (TAG) without complicated pretreatment. We identified a series of CC location isomers via mCPBA-nanoESI-MS/MS, among them, FA 24:1 (Δ13) and FA 24:1 (Δ17) were first identified in edible oils, and the predominant UFAs was FA 18:1 (Δ9), which occupies 98.35% of FA 18:1 in peanut oil while 89.68% in rapeseed oil. The results demonstrated that the proposed method could provide further in-depth CC positional information of oils, promoting the development of structural determination of fatty acids in food chemistry.


Assuntos
Ácidos Graxos não Esterificados , Espectrometria de Massas em Tandem , Ácidos Graxos , Óleos Vegetais , Óleo de Brassica napus
14.
Food Chem ; 375: 131819, 2022 May 01.
Artigo em Inglês | MEDLINE | ID: mdl-34920310

RESUMO

A modified QuEChERS method coupled to chromatography tandem mass spectroscopy was established and used to identify 56 pesticides and 21 metabolites residues in tea samples. The average recoveries for the target compounds ranged from 71% to 109% with RSDs of 1-17%. Pesticides and metabolites residues in 248 tea samples from China were investigated by the developed method, and the dietary intake risk for consumers was estimated. The results showed that 36 pesticides and 14 metabolites were detected with concentrations of 0.0050-7.7 mg/kg. There are unlikely to present a public health concern for Chinese consumers. The acute risk of pesticides would be exaggerated when calculated by the residue level in tea instead of tea infusion. The unauthorized and banned pesticide contributed to the chronic and acute hazard index by 68% and 36%, respectively. The cumulative risk of residual pesticides and their metabolites on human health deserve further attention.


Assuntos
Resíduos de Praguicidas , Praguicidas , Cromatografia Líquida de Alta Pressão , Humanos , Resíduos de Praguicidas/análise , Medição de Risco , Espectrometria de Massas em Tandem , Chá
15.
Food Chem ; 374: 131815, 2022 Apr 16.
Artigo em Inglês | MEDLINE | ID: mdl-34920402

RESUMO

Metal ions are known to influence the course of the Maillard reaction through formation of various complexes such as bis(amino acids), these complexes are known to undergo more facile reaction with sugars. Due to this enhanced reactivity, the possible formation of di-glycated amino acids in glucose/alanine model systems with and without FeCl2 was investigated using isotope labelling technique in conjunction with ESI/qTOF/MS/MS. Forty-eight derivatives of bis[N,N'-di-glycated alanine] iron(II) complexes were tentatively identified. These complexes incorporated one iron atom, two [13C-3] atoms from alanine and up-to twenty-four carbon atoms from glucose [13C-U], were incorporated as triose (C3), tetrose (C4), pentose (C5) or hexose (C6) moieties. Furthermore, the dissociation of the above complexes released variously substituted N,N-di-glycated alanine derivatives incorporating one alanine [13C-3] atom and up to twelve carbon atoms from glucose [13C-U]. The MS/MS analysis of diglycated alanines indicated that they follow similar fragmentation pathways as Amadori product of alanine.


Assuntos
Alanina , Glucose , Compostos Ferrosos , Ferro , Espectrometria de Massas em Tandem
16.
Food Chem ; 374: 131712, 2022 Apr 16.
Artigo em Inglês | MEDLINE | ID: mdl-34920407

RESUMO

Metal-organic frameworks (MOFs) has excellent adsorption performance, herein, three kinds of common MOFs were used for the adsorption of sulfamethazine (SM2) in milk, then enzyme-linked immunosorbent assay (MOF-ELISA) was established. Firstly, NH2-UiO-66, NH2-MIL-101, and ZIF-8 were successfully prepared and their adsorption characteristics for SM2 were investigated. The kinetic models of the three MOFs were more in line with the pseudo-second-order adsorption kinetics, and the saturated adsorption capacity of NH2-UiO-66, NH2-MIL-101, and ZIF-8 for SM2 at 298 K were 139.64, 29.98, and 36.5 mg/g, respectively. Using three different MOFs as adsorbents, the pretreatment of milk samples could be completed within 1 h, the half inhibitory concentrations (IC50) of MOF-ELISA were 1.26, 1.86 and 2.74 ng/mL, the limit of detections (LOD) were 0.05, 0.12, and 0.19 ng/mL and the recovery rate were from 82.30% to 105.62% with the intra-day coefficient of variations (CVs) below 5.81% and inter-day CVs below 7.21%. Detection results showed good correlations with LC-MS/MS (R2 > 0.99), indicated that MOFs could effectively eliminate the interference of sample matrix, and has the potential to become a general pretreatment method for the detection of various matrices residues in food safety monitoring.


Assuntos
Estruturas Metalorgânicas , Adsorção , Animais , Cromatografia Líquida , Ensaio de Imunoadsorção Enzimática , Leite , Ácidos Ftálicos , Sulfametazina , Espectrometria de Massas em Tandem
17.
Food Chem ; 374: 131782, 2022 Apr 16.
Artigo em Inglês | MEDLINE | ID: mdl-34920409

RESUMO

The manuscript reports comprehensive multi-residue determination of 215 pesticides in two commercially important Indian spices, Cumin (Cuminum cyminum) and Coriander (Coriandrum sativum) by GC-MS/MS analysis. The proposed method involved liquid-liquid extraction with acetonitrile, d-SPE clean-up and final reconstitution of extract in ethyl acetate. d-SPE clean-up with PSA and C18 minimized the matrix effects by 40 and 16%, respectively. Reconstitution of final extract reduced the non-volatile matrix co-extractives by 36-40%. The method was validated as per SANTE/12682/2019 and recoveries at 10, 25 and 50 µg kg-1 were within 70-120% with RSD ≤ 20%. A fit for purpose method LOQ of 10 µgkg-1 was achieved for 85% of analytes. The method was successfully applied for comprehensive screening of cumin and coriander market samples. The calculated TMDI for acute and chronic exposure assessment were less than calculated MPI in respective matrices and therefore did not cause any adverse effect to consumers.


Assuntos
Coriandrum , Cuminum , Resíduos de Praguicidas , Cromatografia Gasosa-Espectrometria de Massas , Resíduos de Praguicidas/análise , Extração em Fase Sólida , Especiarias/análise , Espectrometria de Massas em Tandem
18.
Food Chem ; 375: 131891, 2022 May 01.
Artigo em Inglês | MEDLINE | ID: mdl-34952384

RESUMO

The volatility of the vanilla market calls attention to the so-called vanilla crisis. There is a growing worldwide demand for natural vanilla with a concomitant reduction in global supply. However, commercial crops are threatened with extinction due to the lack of gene pool variability, susceptibility to climate change and pandemic diseases. Therefore, there is an urgent need to identify new Vanilla spp. as alternative sources vanilla. Therefore, using undirected LC-MS/MS metabolic profiling and chemometrics, the present study demonstrates the great bioeconomic potential of two Atlantic Forest species - V. bahiana and V. chamissonis - by annotation of important flavor compounds associated with the commercial species and reveals distinct flavor descriptors associated with both wild species. Such similarities and dissimilarities are crucial to the ongoing quest to Vanilla gene pool improvement. Compounds remarkably and frequently associated with vanilla flavor were annotated or identified in this study such as vanillin and p-hydroxybenzaldehyde.


Assuntos
Vanilla , Benzaldeídos , Cromatografia Líquida , Florestas , Espectrometria de Massas em Tandem
19.
Food Chem ; 375: 131726, 2022 May 01.
Artigo em Inglês | MEDLINE | ID: mdl-34954579

RESUMO

A robust and sensitive isotope dilution UPLC-MS/MS method was established for the simultaneous analysis of acrylamide (AA), 5-hydroxymethylfurfural (HMF), and 2-amino-1-methyl-6-phenylimidazo[4,5-b]-pyridine (PhIP). A fairly good separation of three analytes was achieved within 4.5 min. High correlation coefficients (R2 > 0.9998) of the three compounds were obtained in their respective linear ranges. This method demonstrated low limits of detection (1.57 µg/L for AA, 0.61 µg/L for HMF, and 0.02 µg/L for PhIP) and limits of quantification (5.22 µg/L for AA, 2.03 µg/L for HMF, and 0.05 µg/L for PhIP). This method also demonstrated excellent quantification accuracy (99.02%-101.12%), precision (RSD < 6%), and recovery (82.83-119.92%) in the Maillard model systems and deep-fried meatballs. This work develops a fundamental method for the rapid simultaneous determination of AA, HMF, and PhIP in thermally processed foods that are both carbohydrates-rich and protein-rich, meanwhile providing technical support for the generation mechanism of various hazards.


Assuntos
Acrilamida , Espectrometria de Massas em Tandem , Cromatografia Líquida de Alta Pressão , Cromatografia Líquida , Furaldeído/análogos & derivados , Piridinas
20.
Food Chem ; 375: 131894, 2022 May 01.
Artigo em Inglês | MEDLINE | ID: mdl-34954580

RESUMO

A novel strategy for screening and identifying peptides present in Baijiu was developed based on magnetic solid-phase extraction with magnetic S-doped graphene (M-G-S) as adsorbent combined with ultrahigh-performance liquid chromatography with high resolution tandem mass spectrometry. In total, 28 peptides consisting of amino acids from 3 to 9 were preliminarily identified, and significantly higher in the number than that of direct concentration and SPE with C18 as the adsorbent. Six peptides were confirmed with their corresponding synthetic reference standards by comparing their retention time, high resolution MS/MS spectra, and NMR spectroscopic studies. Parallel reaction monitoring integrated with the internal standard method was utilized to quantify identified peptides with concentrations ranging from 1.14 to 10.25 ng mL-1, and prediction results of bioactivity comprising antioxidation or ACE inhibitors were obtained. These discoveries were conducive to understanding the versatility benefit of Baijiu and paved the way to study the interaction between peptides and volatile substances.


Assuntos
Extração em Fase Sólida , Espectrometria de Massas em Tandem , Cromatografia Líquida de Alta Pressão , Cromatografia Líquida , Peptídeos
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