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1.
J Sep Sci ; 44(17): 3199-3207, 2021 Sep.
Artigo em Inglês | MEDLINE | ID: mdl-34213832

RESUMO

A fast and simple ultra-high performance supercritical fluid chromatography method has been developed for the determination of six analytes, namely (paeonol, coumarin, cinnamic alcohol, cinnamic acid, paeoniflorin, and amygdalin) in Guizhi Fuling capsule and tablet samples. The influence of the key chromatographic parameters for the separation purposes was evaluated. The optimal column was Trefoil CEL1 column. The optimal mobile phase was a gradient mixture of carbon dioxide and methanol at flow rate of 1.0 mL/min. The back pressure of the system was set to 1.38 × 107  Pa and the temperature to 45°C. The six compounds were separated within 11 min by the proposed ultra-high performance supercritical fluid chromatography method with satisfactory resolution. Method validation confirmed that the procedure is accurate with the recovery rates from 87.04 to 104.30%, intraday precision values less than 4.81% and interday precision less than 5.22%, and linear with R2 higher than 0.9967. Therefore, this work provides a simple and novel method for the simultaneous analysis of six compounds in Guizhi Fuling capsule and tablet samples.


Assuntos
Medicamentos de Ervas Chinesas/química , Acetofenonas/análise , Amigdalina/análise , Cápsulas/análise , Cromatografia com Fluido Supercrítico , Cinamatos/análise , Cumarínicos/análise , Glucosídeos/análise , Monoterpenos/análise , Propanóis/análise , Comprimidos
2.
Molecules ; 22(9)2017 Aug 30.
Artigo em Inglês | MEDLINE | ID: mdl-28867779

RESUMO

Processing is a traditional pharmacy technology based on traditional Chinese medicine theory. The traditional Chinese medicine (TCM) ingredients should be processed before being used as a medicine. Processed bitter almonds are widely used in the clinic in TCM for the treatment of cough and asthma. In this work the amygdalin profile of three producing areas in China was determined, with respect to three differently processed bitter almond products: raw, stir-fried and scalded. Identification of the compounds was done by using high performance liquid chromatography coupled to electrospray ionization mass spectrometry (HPLC-ESI-MS/MS). Results indicated that amygdalin, neoamygdalin and amygdalin amide were identified in the different processed bitter almonds. Meanwhile, amygdalin was used as a standard to calculate the quantification of amygdalin and the concentration ratio of neoamygdalin and total amygdalin by HPLC-DAD. The data suggested that composition of amygdalin isomers in bitter almonds was influenced by the processing method. It also gives a new understanding of the processing principle of bitter almonds. Moreover, the classification of different processed bitter almonds can be achieved on the basis of amygdalin isomers levels.


Assuntos
Amigdalina/análise , Cromatografia Líquida de Alta Pressão/métodos , Prunus/química , Espectrometria de Massas por Ionização por Electrospray/métodos , Espectrometria de Massas em Tandem/métodos , Amigdalina/química , Isomerismo , Análise de Componente Principal , Reprodutibilidade dos Testes
3.
Phytochem Anal ; 25(2): 122-6, 2014.
Artigo em Inglês | MEDLINE | ID: mdl-24115144

RESUMO

INTRODUCTION: Prunus serotina is native to North America but has been invasively introduced in Europe since the seventeenth century. This plant contains cyanogenic glycosides that are believed to be related to its success as an invasive plant. For these compounds, chromatographic- or spectrometric-based (targeting on HCN hydrolysis) methods of analysis have been employed so far. However, the conventional methods require tedious preparation steps and a long measuring time. OBJECTIVE: To develop a fast and simple method to quantify the cyanogenic glycosides, amygdalin and prunasin in dried Prunus serotina leaves without any pre-purification steps using (1) H-NMR spectroscopy. METHODS: Extracts of Prunus serotina leaves using CH3 OH-d4 and KH2 PO4 buffer in D2 O (1:1) were quantitatively analysed for amygdalin and prunasin using (1) H-NMR spectroscopy. Different internal standards were evaluated for accuracy and stability. The purity of quantitated (1) H-NMR signals was evaluated using several two-dimensional NMR experiments. RESULTS: Trimethylsilylpropionic acid sodium salt-d4 proved most suitable as the internal standard for quantitative (1) H-NMR analysis. Two-dimensional J-resolved NMR was shown to be a useful tool to confirm the structures and to check for possible signal overlapping with the target signals for the quantitation. Twenty-two samples of P. serotina were subsequently quantitatively analysed for the cyanogenic glycosides prunasin and amygdalin. CONCLUSION: The NMR method offers a fast, high-throughput analysis of cyanogenic glycosides in dried leaves permitting simultaneous quantification and identification of prunasin and amygdalin in Prunus serotina.


Assuntos
Amigdalina/análise , Glicosídeos/análise , Espectroscopia de Ressonância Magnética/métodos , Nitrilas/análise , Extratos Vegetais/análise , Prunus/química , Amigdalina/química , Amigdalina/isolamento & purificação , Glicosídeos/química , Glicosídeos/isolamento & purificação , Hidrogênio/análise , Nitrilas/química , Nitrilas/isolamento & purificação , Extratos Vegetais/química , Extratos Vegetais/isolamento & purificação , Folhas de Planta/química , Propionatos/normas , Padrões de Referência , Reprodutibilidade dos Testes , Sensibilidade e Especificidade , Fatores de Tempo , Compostos de Trimetilsilil/normas
4.
Zhongguo Zhong Yao Za Zhi ; 38(5): 687-90, 2013 Mar.
Artigo em Chinês | MEDLINE | ID: mdl-23724676

RESUMO

OBJECTIVE: To establish an HPLC method for the determination of ephedrine hydrochloride, D-pseudo-ephedrine and amygdalin in Xiao'er Pingchuan Qutan granule. METHOD: Pheny ether chromatographic column (4.6 mm x 250 mm, 5 microm) was adopted, with acetonitrile-0.1% phosphoric acid (containing 0.1% three ethylamine) (3:97) as the mobile phase. The UV detection wavelength was at 210 nm, with the flow rate of 1 mL x min(-1), and column temperature was at 35 degrees C. RESULT: The linearity of ephedrine hydrochloride, D-pseudo-ephedrine and amygdalin ranged between 0.078 60-3.144 microg (r = 1.000 0), 0.103 4-2.068 microg (r = 0.999 7) and 0.430 5-3.157 microg (r = 0.999 8), respectively. Their average recoveries were 98.46% (RSD 1.1%), 103.0% (RSD 1.5%) and 97.15% (RSD 2.1%), respectively. CONCLUSION: The method is simple, stable and reliable that it can be used to determine the content of ephedrine hydrochloride, D-pseudo-ephedrine and amygdalin in Xiao'er Pingchuan Qutan granule.


Assuntos
Amigdalina/análise , Medicamentos de Ervas Chinesas/química , Efedrina/análise , Pseudoefedrina/análise , Amigdalina/química , Cromatografia Líquida de Alta Pressão , Efedrina/química , Modelos Lineares , Pseudoefedrina/química , Reprodutibilidade dos Testes , Fatores de Tempo
5.
Food Res Int ; 164: 112437, 2023 02.
Artigo em Inglês | MEDLINE | ID: mdl-36738016

RESUMO

Valorizing food wastes and by-products can improve economic and environmental sustainability of the food production chain. In this regard, Meghalayan cherry kernels are a good source of proteins, but the presence of toxic compounds like amygdalin, makes them underutilized. Therefore, the present study was focused on detoxifying Meghalayan cherry kernel using thermal, soaking and ultrasound treatments and studying their impact on the structural and thermal characteristics of protein isolate. The results showed that all three treatments significantly reduced amygdalin content, with complete detoxification achieved after 30 and 60 min at 70 °C and 60 °C, respectively, in ultrasound, and after 90 and 120 min at 70 °C and 60 °C, respectively, in soaking + thermal treatment. The detoxification treatments significantly affected the protein content and weight-loss of Meghalayan cherry kernel. Fluorescence spectroscopy and FTIR showed alterations in Meghalayan cherry kernel protein isolate (MCKPI) secondary and tertiary structure. The fluorescence intensity was observed at 340 nm for native and detoxified protein isolate, and the lowest peak for MCKPI-US depicts conformational changes. The fading of bands in SDS-PAGE confirms structural changes due to thermal and sonication effects. SEM images demonstrated that more cracks and porous structures were seen in treated MCKPI than native MCKPI. Detoxification treatment increased thermal stability, resulting in lesser weight loss and higher denaturation temperature than native MCKPI. In this study, ultrasound treatment demonstrated the most pronounced effects on the detoxification of MCKPI and its thermal and structural properties, suggesting that Meghalayan cherry kernel is one of the most promising substrates for zero-waste bioprocess development.


Assuntos
Amigdalina , Prunus , Sementes/química , Amigdalina/análise , Temperatura Alta
6.
J Chromatogr Sci ; 61(2): 110-118, 2023 Feb 03.
Artigo em Inglês | MEDLINE | ID: mdl-35396599

RESUMO

Bitter almond is a well-known and commonly used traditional Chinese medicine (TCM) for relieving coughs and asthma. However, the bioactive chemical composition of bitter almonds, especially their amygdalin content, which determines their quality for TCM use, is variable and this can cause problems with formulating and prescribing TCMs based on bitter almonds. Therefore, a simple method was developed to evaluate the compositional quality of bitter almonds from their appearance traits, based on a combination of chromatographic fingerprinting and chemometrics. Bitter almonds were analyzed by high-performance liquid chromatography (HPLC). Hierarchical cluster analysis (HCA) and principal components analysis (PCA) were applied to classify bitter almonds, which split the samples into two independent clusters. Three chemical markers (amygdalin, prunasin, and one unidentified component) were found by partial least squares-discriminant analysis (PLS-DA). What's more, a new PLS-DA model was reconstructed to confirm the obtained chemical markers from PLS-DA. Additionally, the appearance trait indices and amygdalin content of bitter almond were determined and the classification was confirmed by one-way analysis of variance. This method can easily determine the quality of bitter almonds from their appearance alone, high quality correlated closely with kernels that were larger, oblong in shape and heavier.


Assuntos
Amigdalina , Prunus dulcis , Amigdalina/análise , Amigdalina/química , Quimiometria , Cromatografia Líquida de Alta Pressão/métodos , Medicina Tradicional Chinesa , Análise de Componente Principal
7.
J AOAC Int ; 106(2): 457-463, 2023 Mar 01.
Artigo em Inglês | MEDLINE | ID: mdl-36453858

RESUMO

BACKGROUND: Cyanogenic glycosides are secondary metabolites in plants. In almonds and apricot kernels, amygdalin is an abundant cyanogenic glycoside. Upon consumption, amygdalin is enzymatically metabolized into hydrogen cyanide. Depending on the number of kernels consumed and the amygdalin concentration, ingestion of amygdalin-containing kernels may result in adverse effects. To better understand the US marketplace, the development and validation of analytical methods to reliably measure amygdalin in apricot kernels and almonds is needed to support the collection of occurrence and consumption data in retail products. OBJECTIVE: The aim of this study was to develop and validate a liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for the quantitation of amygdalin in apricot kernels and almonds following the U.S. Food and Drug Administration (FDA). Foods Program Guidelines for the Validation of Chemical Methods, 3rd Edition. METHODS: Apricot kernels and almonds were cryogenically homogenized and extracted using methanol containing an internal standard (IS), geniposide, followed by filtration, dilution, and LC-MS/MS analysis. Matrix effects were minimized using dilution. Quantitation was achieved using an external, solvent-based calibration. RESULTS: The amygdalin response was linear (r2 > 0.99) over a range of 0.05-50 µg/mL. The recovery of amygdalin spiked at 10-10 000 µg/g in sweet apricot kernels, raw almond, and dry-roasted almond ranged from 90 to 107% with RSDs ≤6%. The method limit of detection and limit of quantitation was 0.8 and 2.5 ng/g, respectively. Amygdalin concentrations in 18 market samples ranged from 2 to 24 000 µg/g. Corresponding estimates of cyanide concentration ranged from 0.2 to 1420 µg/g. CONCLUSIONS: Method performance meets the acceptance criteria defined by FDA guidelines and is fit for purpose for the analysis of amygdalin in apricot kernels and almonds. HIGHLIGHTS: An LC-MS/MS method is developed for the quantification of amygdalin in apricot kernels and almonds.


Assuntos
Amigdalina , Prunus armeniaca , Prunus dulcis , Amigdalina/análise , Amigdalina/química , Amigdalina/metabolismo , Prunus armeniaca/química , Cromatografia Líquida , Espectrometria de Massas em Tandem/métodos
8.
Molecules ; 17(11): 12925-37, 2012 Nov 01.
Artigo em Inglês | MEDLINE | ID: mdl-23117432

RESUMO

A high performance liquid chromatographic (HPLC) method with diode array detection (DAD) was established for simultaneous determination of seven main bioactive components in San-ao decoction and its series of formulae (San-ao decoction, Wu-ao decoction, Qi-ao decoction and Jia-wei San-ao decoction). Seven compounds were analyzed simultaneously with a XTerra C(18) column (4.6 mm × 250 mm, 5 µm) using a linear gradient elution of a mobile phase containing acetonitrile (A) and a buffer solution (0.02 mol/L potassium dihydrogen phosphate and adjusted to pH 3 using phosphoric acid) (B); the flow rate was 1.0 mL/min. The sample was detected with DAD at 210, 254 and 360 nm and the column was maintained at 30 °C. All the compounds showed good linearity (r2 > 0.9984) in the tested concentration range. The precisions were evaluated by intra-day and inter-day tests, and relative standard deviation (R.S.D.) values within the range of 0.83%–2.53% and 0.64%–2.77% were reported, respectively. The recoveries of the quantified compounds were observed to cover a range from 95.34% and 104.82% with R.S.D. values less than 2.72%. The validated method was successfully applied for the simultaneous determination of seven main bioactive components including ephedrine (1), amygdalin (2), liquiritin (3), benzoic acid (4), isoliquiritin (5), formononetin (6) and glycyrrhizic acid (7) in San-ao decoction and its series of formulae. The results also showed a wide variation in the content of the identified active compounds in these samples, which could also be helpful to illustrate the drug interactions after some herbs combined in different formulations.


Assuntos
Medicamentos de Ervas Chinesas/análise , Amigdalina/análise , Amigdalina/química , Amigdalina/isolamento & purificação , Ácido Benzoico/análise , Ácido Benzoico/química , Ácido Benzoico/isolamento & purificação , Calibragem , Chalcona/análogos & derivados , Chalcona/análise , Chalcona/química , Chalcona/isolamento & purificação , Cromatografia Líquida de Alta Pressão/normas , Medicamentos de Ervas Chinesas/química , Medicamentos de Ervas Chinesas/isolamento & purificação , Efedrina/análise , Efedrina/química , Efedrina/isolamento & purificação , Flavanonas/análise , Flavanonas/química , Flavanonas/isolamento & purificação , Glucosídeos/análise , Glucosídeos/química , Glucosídeos/isolamento & purificação , Ácido Glicirrízico/análise , Ácido Glicirrízico/química , Ácido Glicirrízico/isolamento & purificação , Isoflavonas/análise , Isoflavonas/química , Isoflavonas/isolamento & purificação , Limite de Detecção , Medicina Tradicional Chinesa , Padrões de Referência , Razão Sinal-Ruído , Espectrofotometria Ultravioleta/normas
9.
Chemosphere ; 307(Pt 4): 136061, 2022 Nov.
Artigo em Inglês | MEDLINE | ID: mdl-35977575

RESUMO

Consumption of fermented Prunus mume fruit (maesil) sugar syrup raise a health concern due to the presence of the cyanogenic glucoside amygdalin. The goal of the present study was to investigate the amygdalin degradation potential and genome profile of the native microbes found in maesil syrup. The microbial profile analysis revealed that yeast is the predominant microorganism native to maesil syrup and that the isolated yeast cells showed a remarkable potential for amygdalin reduction (99.7%). Moreover, the reduction in amygdalin was inversely proportional to the growth of the isolated yeast. The whole-genome analysis revealed that the isolated yeast is Zygosaccharomyces rouxii (genome size 10 Mb, 39.25% of GC content). Of the 5250 genes (64.88%) predicted in the Z. rouxii genome, 5245 (99.90%) were annotated using NCBI Non-Redundant, UniProt, and InterProScan databases. The genome of the isolated Z. ruoxii harbored 2.03% of repeats and 0.68% of non-coding RNAs. Protein prediction indicated that ß-glycosidases and hydroxynitrile lyase may play a key role in amygdalin degradation. The predicted degradation initiated by ß-glycosidases that hydrolyze α-glucosidic bonds of amygdalin results in α-hydroxy nitriles (cyanohydrins) that are subsequently converted into carbonyl compounds (benzaldehyde) and hydrogen cyanide catalyzed by hydroxynitrile lyases. Present findings provide valuable data for constructing engineered microorganisms that can degrade amygdalin. Further analysis of Z. rouxii may elucidate the exact mechanism of amygdalin reduction in the production of maesil syrup.


Assuntos
Amigdalina , Prunus , Amigdalina/análise , Amigdalina/química , Amigdalina/metabolismo , Benzaldeídos/análise , Frutas/química , Glucosídeos , Glicosídeo Hidrolases , Glicosídeos , Cianeto de Hidrogênio/análise , Nitrilas/química , Prunus/química , Prunus/metabolismo , Saccharomyces cerevisiae/metabolismo , Açúcares
10.
Electrophoresis ; 32(2): 218-22, 2011 Jan.
Artigo em Inglês | MEDLINE | ID: mdl-21254118

RESUMO

A new method for separation and determination of amygdalin and its epimer (neoamygdalin) in the epimerization of amygdalin by MEEKC is proposed. For the chiral separation of amygdalin and neoamygdalin, a running buffer composed of 80 mM sodium cholate, 5.0% v/v butan-1-ol, 0.5% v/v heptane and 94.5% v/v 30 mM Na(2) B(4) O(7) buffer (pH 9.00) is proposed. Under optimum conditions, the basic separation of amygdalin and neoamygdalin can be achieved within 7 min. The calibration curve for amygdalin showed excellent linearity in the concentration range of 20-1000 µg/mL with a detection limit of 5.0 µg/mL (S/N=3). The epimerization rate constant of amygdalin in basic microemulsion was first determined by monitoring the concentration changes of amygdalin, and the epimerization rate constant of amygdalin was found to be 2×10(-3) min(-1) at 25°C under the above optimum microemulsion conditions.


Assuntos
Amigdalina/química , Eletrocromatografia Capilar/métodos , Amigdalina/análise , Soluções Tampão , Emulsões/química , Cinética
11.
J AOAC Int ; 93(2): 478-84, 2010.
Artigo em Inglês | MEDLINE | ID: mdl-20480892

RESUMO

A reference method (higher accuracy) and a routine method (higher throughput) were developed for the extraction of cyanogenic glycosides from flaxseed. Conditions of (essentially) complete extraction were identified by comparing grinding methods and extraction solvent composition, and optimizing solvent-to-meal ratio, extraction time, and repeat extraction. The reference extraction method consists of sample grinding using a high-speed impact plus sieving mill at 18 000 rpm with a 1.0 mm sieve coupled with triple-pooled extraction in a sonicating water bath (40 degrees C, 30 min) using 75% methanol. The routine method differs by the use of a coffee mill to grind samples and a single extraction. The 70 and 80% methanol solutions were equal and superior to other combinations from 50 to 100% aqueous ethanol or methanol. The extraction efficiencies of the routine method (relative to the reference method) was 87.9 +/- 2.0% SD (linustatin) and 87.6 +/- 1.9% SD (neolinustatin) using four composite samples that were generated from seeds of multiple cultivars over two crop years and locations across Western Canada. Ground flaxseed was stable after storage at room temperature, refrigeration, or freezing for up to 7 days, and frozen for at least 2 weeks but less than 2 months. Extracts were stable for up to 1 week at room temperature and at least 2 weeks when refrigerated or frozen.


Assuntos
Amigdalina/análogos & derivados , Linho/química , Análise de Alimentos/métodos , Glicosídeos/análise , Glicosídeos/isolamento & purificação , Amigdalina/análise , Amigdalina/isolamento & purificação , Técnicas de Química Analítica , Cromatografia Gasosa/instrumentação , Cromatografia Gasosa/métodos , Etanol/química , Metanol/química , Valores de Referência , Reprodutibilidade dos Testes , Solubilidade , Solventes/química , Temperatura , Fatores de Tempo
12.
Zhongguo Zhong Yao Za Zhi ; 35(20): 2684-8, 2010 Oct.
Artigo em Chinês | MEDLINE | ID: mdl-21246818

RESUMO

OBJECTIVE: To study the influence of processing on metabolism of the main component of bitter almond-amygdalin in rat. METHOD: The blood was collected at different times after amygdalin given by injection and oral, bitter almond and its processed production given by oral respectively, and then detected by both HPLC and HPLC-MS(n) methods after extraction pretreatment. RESULT: After injection, amygdalin was absorbed in prototype to blood rapidly, while the other three kinds of medicine given by oral were all not detected the prototype of amygdalin, but two metabolites were detected which were isomers of prunasin confirmed by mass spectrometry. The metabolic pathway of prunasin in processed bitter almond group was markedly different from the bitter almond group. CONCLUSION: Processing has a significant effect on bitter almond metabolic processes in rats.


Assuntos
Amigdalina/metabolismo , Prunus/química , Amigdalina/análise , Animais , Feminino , Masculino , Ratos , Ratos Sprague-Dawley
13.
Artigo em Inglês | MEDLINE | ID: mdl-32618500

RESUMO

Amygdalin, prunasin, total cyanide and free cyanide concentrations in 12 powdered loquat seeds were investigated. Loquat (Eriobotrya japonica) is a species of flowering plant in the family Rosaceae, and its fruit is quite popular in Japan. Amygdalin and prunasin were measured using LC-MS/MS. Total cyanide was measured by enzymatic treatment, steam distillation and colorimetric quantification using the pyridine-pyrazolone method. Free cyanide was measured without enzymatic treatment. The mean concentrations of amygdalin, prunasin, total cyanide and free cyanide in powdered loquat seeds were 5900, 760, 410 and 44 mg/kg, respectively. The range of each quantitative value was extensive. Seven out of twelve samples were at risk for exceeding the acute reference dose (ARfD) of cyanide.


Assuntos
Amigdalina/análise , Cianetos/análise , Eriobotrya/química , Nitrilas/análise , Pós/química , Sementes/química , Cromatografia Líquida , Espectrometria de Massas em Tandem
14.
Anticancer Agents Med Chem ; 20(7): 897-908, 2020.
Artigo em Inglês | MEDLINE | ID: mdl-32167430

RESUMO

Indroduction: This article presents a theoretical analysis of the safe form and dosage of the amygdalin derivative. By making a precise socio-anthropological analysis of the life of the ancient people of Botra (Hunza people, Burusho/Brusho people), a hypothesis has been postulated through a number of modern quantum-mechanical, molecular-topological and bio analytical checks, and has also been confirmed by two proofs. METHODS: The proposed hypothesis underwent theoretical and logical analysis to confirm and/or reject it. The methodological scheme was: determining the optimal chemical formula, determination of the pharmaceutical molecular form and determination of the drug dose. RESULTS: A convenient, harmless, form of amygdalin derivative is available that has the same biological and chemical activity and could be used in conservative clinical oncology. The article also presents a theoretical comparative analysis of biochemical reactivity in in vivo and in vitro media, by which we also determine the recommended dosage for patient administration. A comparative analysis of the data, obtained in published clinical studies of amygdalin, is presented, summarizing a scheme of the anti-tumor activity of the proposed molecular form. CONCLUSION: The hydrolyzed to amide / carboxylic acid cyano / nitrile glycosides are potential drugs. Their biological activity remains unchanged, but their toxicity is many times lower than unmodified native molecules. We claim that this study we have conducted on amygdalin / dhurrin-derived amide is the only study on this molecular form. Other substances in these groups with pronounced biological activity (including anti-tumor) are the hydrolyzed nitrile groups by Prunasin, Lucumin, Vicianin, Sambunigrin, Dhurrin, Taxiphyllin, Zierin, Preteacin, p-Glucosyloxymandelonitrile, Linamarin, Lotaustralin, Acaciapetalin, Triglochinin, Dejdaclin, Tetraphyllin A, Tetrallin B, Gynocardin etc., to their amide/carboxylic acid.


Assuntos
Amigdalina/análise , Antineoplásicos Fitogênicos/análise , Neoplasias/tratamento farmacológico , Adolescente , Adulto , Idoso , Idoso de 80 Anos ou mais , Amigdalina/análogos & derivados , Amigdalina/uso terapêutico , Antineoplásicos Fitogênicos/uso terapêutico , Relação Dose-Resposta a Droga , Feminino , Humanos , Masculino , Pessoa de Meia-Idade , Conformação Molecular , Adulto Jovem
15.
Food Addit Contam Part B Surveill ; 13(3): 155-161, 2020 Sep.
Artigo em Inglês | MEDLINE | ID: mdl-32207373

RESUMO

There is scarce data on the mycotoxin profile in retailed fruit juices in Nigeria. Thirty-five industrially-processed fruit juice samples randomly purchased from retailers in Ogun state, Nigeria, were analysed for the presence of > 650 toxic fungal and plant metabolites using a liquid chromatography tandem mass spectrometric method. Only 18 metabolites, including 3-nitropropionic acid, alternariol methylether and emodin, but excluding citrinin, fumonisin B2, ochratoxin A and patulin, were detected in trace levels in at least one juice sample. Amygdalin, a plant cyanogen, was quantified (2.05-359 µg/L) in 40% of the samples. Although the levels of mycotoxins and toxic plant metabolites found in the juice may be relatively low, daily consumption of juices containing such low levels may contribute to dietary exposures to these natural chemical contaminants in consumers. Fruit juice processors should be encouraged to adhere strictly to good manufacturing practices in order to keep mycotoxins away from the final products.


Assuntos
Contaminação de Alimentos/análise , Sucos de Frutas e Vegetais/análise , Frutas/química , Fungos , Micotoxinas/análise , Plantas/química , Amigdalina/análise , Cromatografia Líquida/métodos , Comércio , Dieta , Emodina/análise , Frutas/microbiologia , Fungos/crescimento & desenvolvimento , Humanos , Nitrocompostos/análise , Patulina/análise , Plantas/microbiologia , Propionatos/análise , Espectrometria de Massas em Tandem/métodos
16.
Artigo em Inglês | MEDLINE | ID: mdl-31397641

RESUMO

This work is focused on separation and determination of amygdalin and its unnatural form neoamygdalin in natural food supplements. Reversed-phase high-performance liquid chromatography with a high-stability silica-based column with C18 functional group has been used for solving this problem. The effect of the mobile phase composition as well as the column temperature on the separation of the amygdalin epimers has been investigated. Isocratic elution using a mobile phase composed of 0.05% aqueous formic acid and acetonitrile achieved the required separation within 17 min. Under optimum chromatographic conditions, the developed method was validated and was applied for the determination of amygdalin epimers in natural food supplements containing apricot or peach kernels. A simple extraction method using methanol as an extractant supported by an ultrasonic bath was used with recovery in the range of 94.8% to 104.3%. The limit of detection and limit of quantification values for R-amygdalin were 0.13 mg/L and 0.40 mg/L, respectively. The developed method proved to be precise with the intra-day and inter-day relative standard deviation values less than 2.23%.


Assuntos
Amigdalina/análise , Antineoplásicos Fitogênicos/análise , Suplementos Nutricionais/análise , Análise de Alimentos , Contaminação de Alimentos/análise , Dióxido de Silício/química , Cromatografia Líquida de Alta Pressão , União Europeia , Conformação Molecular
17.
J Chromatogr A ; 1601: 214-223, 2019 Sep 13.
Artigo em Inglês | MEDLINE | ID: mdl-31076224

RESUMO

An ultra performance liquid chromatography electrospray ionization high-resolution mass spectrometry (UPLC/ESI-HRMS) method was developed and validated for simultaneous quantification of cyanogenic glycosides (CGs), [linustatin (LIS) and neolinustatin (NLIS)], and the main lignan, secoisolariciresinol diglucoside (SDG) in Linoforce® (LF) [flaxseed (Linum usitatissimum L.) coated with two herbal extracts (Senna alexandrina mill and Frangula alnus)]. CGs and SDG were extracted from defatted ground LF by a new procedure consisting of an aqueous methanol ultrasound-assisted extraction followed by an aqueous alkaline ultrasound-assisted extraction of the residue. The combined extracted solutions were then hydrolyzed by 0.02 M NaOH to release SDG from its hydroxymethyl glutaryl ester-linked complex (SDG-HMG). After hydrolysis, the sample was acidified and analyzed directly, without the need of any additional clean-up steps, by UPLC/ESI-HRMS in positive mode. The identification of CGs and SDG was confirmed by the similar retention time and similar MS spectra to the corresponding authentic standards. The quantification was performed using the corresponding extracted ion chromatograms and amygdalin as internal standard. The overall method was validated in terms of linearity, stability, selectivity, precision and accuracy. The developed method was successfully applied to the quantification of CGs and SDG in LF and also in non-coated flaxseed. This is the first report on the simultaneous quantification of CGs and SDG in LF and flaxseed.


Assuntos
Butileno Glicóis/análise , Técnicas de Química Analítica/métodos , Cromatografia Líquida de Alta Pressão , Linho/química , Glucosídeos/análise , Glicosídeos/análise , Espectrometria de Massas , Amigdalina/análogos & derivados , Amigdalina/análise , Hidrólise , Lignanas/análise , Sementes/química
18.
Ultrason Sonochem ; 58: 104614, 2019 Nov.
Artigo em Inglês | MEDLINE | ID: mdl-31450302

RESUMO

Ultrasound has been regarded as an efficient novel technique for debitterizing of the apricot kernels, but its influence is severely concerned on the possible epimerization of d-amygdalin to the l-amygdalin, a more potentially toxigenic compound. Considering this, the experiments were conducted to investigate the epimerization of d-amygdalin and the volatile components in the debitterizing water, which were separated and identified by the high performance liquid chromatography (HPLC) and gas chromatography with a mass spectrometer (GC-MS), respectively. The results indicate that the ultrasonically-debitterizing did not cause the epimerization of d-amygdalin to the l-amygdalin, while the procedure can be greatly accelerated due to the rapid mass transfer and degradation of d-amygdalin induced by ultrasound irradiation. In addition, the water from the ultrasonically-debitterizing of apricot kernels exerted more aromas compared with that of the conventional debitterizing, which might have more applications about this kind of water. In a word, ultrasound can be safely applied in the debitterizing industry of apricot kernels.


Assuntos
Amigdalina/análise , Manipulação de Alimentos , Prunus armeniaca/química , Paladar , Ondas Ultrassônicas , Compostos Orgânicos Voláteis/análise , Amigdalina/química , Amigdalina/metabolismo , Indústria Alimentícia , Estereoisomerismo , Água/química , beta-Glucosidase/metabolismo
19.
J Food Prot ; 71(10): 2048-52, 2008 Oct.
Artigo em Inglês | MEDLINE | ID: mdl-18939751

RESUMO

Amygdalin (laterile) is a cyanogenic glycoside commonly found in the pits of many fruits and raw nuts. When amygdalin-containing seeds are crushed and moistened, free cyanide is formed. Pits and nuts containing unusually high levels of amygdalin can therefore cause cyanide poisoning, and detection of amygdalin in food extracts can be a life-saving measure. In this study, we generated recombinant antibodies against amygdalin from a phage display of a combinatorial rabbit/human chimeric antibody library and used it in a sensitive competition enzyme immunoassay system to detect amygdalin in extracts of pits and nuts. The detection limit was determined to be 1 x 10(-9) M.


Assuntos
Amigdalina/análise , Amigdalina/imunologia , Contaminação de Alimentos/análise , Nozes/química , Sementes/química , Amigdalina/toxicidade , Animais , Doenças Transmitidas por Alimentos/prevenção & controle , Frutas/química , Humanos , Técnicas Imunoenzimáticas/métodos , Coelhos
20.
Phytomedicine ; 45: 68-75, 2018 Jun 01.
Artigo em Inglês | MEDLINE | ID: mdl-29699843

RESUMO

BACKGROUND: Nowadays, to research and formulate an efficiency extraction system for Chinese herbal medicine, scientists have always been facing a great challenge for quality management, so that the transitivity of Q-markers in quantitative analysis of TCM was proposed by Prof. Liu recently. In order to improve the quality of extraction from raw medicinal materials for clinical preparations, a series of integrated mathematic models for transitivity of Q-markers in quantitative analysis of TCM were established. Buyanghuanwu decoction (BYHWD) was a commonly TCMs prescription, which was used to prevent and treat the ischemic heart and brain diseases. In this paper, we selected BYHWD as an extraction experimental subject to study the quantitative transitivity of TCM. STUDY DESIGN: Based on theory of Fick's Rule and Noyes-Whitney equation, novel kinetic models were established for extraction of active components. Meanwhile, fitting out kinetic equations of extracted models and then calculating the inherent parameters in material piece and Q-marker quantitative transfer coefficients, which were considered as indexes to evaluate transitivity of Q-markers in quantitative analysis of the extraction process of BYHWD. METHODS: HPLC was applied to screen and analyze the potential Q-markers in the extraction process. Fick's Rule and Noyes-Whitney equation were adopted for mathematically modeling extraction process. Kinetic parameters were fitted and calculated by the Statistical Program for Social Sciences 20.0 software. The transferable efficiency was described and evaluated by potential Q-markers transfer trajectory via transitivity availability AUC, extraction ratio P, and decomposition ratio D respectively. The Q-marker was identified with AUC, P, D. RESULTS: Astragaloside IV, laetrile, paeoniflorin, and ferulic acid were studied as potential Q-markers from BYHWD. The relative technologic parameters were presented by mathematic models, which could adequately illustrate the inherent properties of raw materials preparation and affection of Q-markers transitivity in equilibrium processing. AUC, P, D for potential Q-markers of AST-IV, laetrile, paeoniflorin, and FA were obtained, with the results of 289.9 mAu s, 46.24%, 22.35%; 1730 mAu s, 84.48%, 1.963%; 5600 mAu s, 70.22%, 0.4752%; 7810 mAu s, 24.29%, 4.235%, respectively. CONCLUSION: The results showed that the suitable Q-markers were laetrile and paeoniflorin in our study, which exhibited acceptable traceability and transitivity in the extraction process of TCMs. Therefore, these novel mathematic models might be developed as a new standard to control TCMs quality process from raw medicinal materials to product manufacturing.


Assuntos
Biomarcadores Farmacológicos/análise , Medicamentos de Ervas Chinesas/química , Modelos Teóricos , Amigdalina/análise , Fracionamento Químico , Cromatografia Líquida de Alta Pressão , Ácidos Cumáricos/análise , Medicamentos de Ervas Chinesas/análise , Glucosídeos/análise , Cinética , Monoterpenos/análise , Saponinas/análise , Triterpenos/análise
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