Probing the degradation of pharmaceuticals in urine using MFC and studying their removal efficiency by UPLC-MS/MS / 药物分析学报

Nutrient recovery from source-separated human urine has attracted interest as it is rich in nitrogen and phosphorus that can be utilized as fertilizer.However,urine also contains pharmaceuticals,steroid hormones,etc.and their removal is crucial as they have detrimental effects on the environment and human health.The current study focuses on investigating the degradation of pharmaceuticals using a double-chamber microbial fuel cell (MFC).Urine was spiked with four pharmaceuticals (trimethoprim,lamivudine,levofloxacin,and estrone) at a concentration of 2 μg/mL.The MFC was operated for 7 months in batch mode with this spiked urine as feed.The degradation efficiency of the MFC was studied,for which a selective liquid chromatography-tandem mass-spectrometric method was developed for the quantitation of compounds used in the spiking experiments and was validated with a lower limit of quantification of 0.39 ng/mL.The maximum removal rate achieved was 96％± 2％.The degradation mechanism involved processes like sorption and anoxic biodegradation.The voltage curve obtained showed that the presence of pharmaceuticals had an initial negative impact on power generation along with increased organic content;however,after the reactor acclimatization,increased power output was achieved with maximum organics removal at 30 h of retention time.This work opens a new perspective for the anoxic biodegradation of pharmaceuticals and can be useful in future bioremediation studies.

Characterization of a novel antifungal protein from Acacia senegal seeds

Aim: The aim of the present study was to isolate antifungal protein from seeds of Acacia senegal in order to develop a new, effective and environmental friendly biofungicide.Methodology: Antifungal protein from A. senegal seeds was extracted and purified through ammonium sulphate precipitation, dialysis, ion exchange and gel filtration chromatography. The novel antifungal was characterized employing SDS-PAGE, chitinase activity and antifungal efficacy. The purified protein was also characterized through MALDI-TOF MS/MS. Results: The yield of purified antifungal protein was estimated to be 0.96 mg 25 g-1 seeds and its molecular mass determined by SDS PAGE was 52.9 kDa. The purified protein exhibited antifungal activity against phytopathogenic fungi viz., Macrophomina phaseolina and Fusarium oxysporum also possessed chitinase activity. The purified protein was characterized through MALDI-TOF MS/MS and its spectra revealed 14 peptides with their specific amino acid sequences. Interpretation: The antifungal protein isolated from A. senegal seeds has broad-spectrum antifungal activity with chitinase activity against pathogenic fungi that can be exploited for management of fungal disease as biopesticide to promote sustainable agriculture

Prevalence of Vitamin D Deficiency Among Newborns

We observed that 760 (92.1%) out of 825 healthy newborns atour institution had vitamin D deficiency (VDD) at birth. Theseobservations highlight the importance of regular screening andsupplementation of vitamin D in the early years of life.

Analysis of molecular changes induced by mineral trioxide aggregate on spla2

Abstract The aim of this study was to analyze the effects of MTA on the structure and enzymatic activity of sPLA2 in order to provide subsidies for improvement in the formulation of the product. MTA powder was incubated for 60 min in the presence of sPLA2 and was analyzed by chromatography, electrospray mass (ESI-MS) and small-angle X-ray scattering (SAXS). It was find that the elution profile, retention time, and fragmentation of sPLA2 were altered after treatment with MTA. Calcium was the MTA component that most amplified the inflammatory signal. Significant interactions were found between MTA and sPLA2, which could aid in our understanding of the mechanisms of action of MTA during the inflammatory process and it may facilitate the structural modification of MTA, thereby improving its biological safety and consequently the rate of the treatment success.

Resumo O objetivo deste estudo foi analisar os efeitos do MTA na estrutura e atividade enzimática da sPLA2 a fim de fornecer subsídios para melhoria na formulação do produto. O MTA em pó foi incubado por 60 min na presença de sPLA2 e analisado por cromatografia, espectroscopia de massa por eletropulverização (ESI-MS) e espalhamento de raios-X de baixo ângulo (SAXS). Encontrou-se que o perfil de eluição, o tempo de retenção e a fragmentação da sPLA2 foram alterados após o tratamento com MTA. O cálcio foi o componente do MTA que mais ampliou o sinal inflamatório. Encontraram-se interações significativas entre o MTA e o sPLA2, o que poderia auxiliar na compreensão dos mecanismos de ação do MTA durante o processo inflamatório e facilitar a modificação estrutural do MTA, melhorando sua segurança biológica e consequentemente a taxa de sucesso do tratamento.

Estudio metabolómico de la enfermedad renal crónica: del modelo experimental al humano / Metabolomics in chronic kidney disease: from experimental model to human disease

Con una prevalencia global reportada de entre 11-13%, la enfermedad renal crónica (ERC) ha sido reconocida como un gran desafío para los sistemas de salud por sus implicaciones económicas y sociales. Al tratarse de una enfermedad crónica e irreversible, el tratamiento está dirigido a disminuir su progresión. La cuantificación de creatinina sérica es el método de elección para su diagnóstico y clasificación; sin embargo, es conocido que esta prueba tiene una sensibilidad clínica limitada, lo que ha conducido a la búsqueda de nuevos marcadores que permitan un diagnóstico y monitoreo oportuno. Desde esta perspectiva, el empleo de la metabolómica y de modelos animales ha permitido la identificación y estudio de nuevos metabolitos, candidatos a ser utilizados como futuros biomarcadores en la práctica clínica. La presente revisión tuvo como objetivo hacer una análisis de los perfiles metabolómicos reportados para la ERC, tanto en modelos experimentales como en estudios realizados en seres humanos. De acuerdo a los datos obtenidos, los metabolitos implicados en las rutas metabólicas de aminas cuaternarias y aminoácidos como el TMNO, el indoxilsulfato y derivados de la dimetilarginina representan una alternativa prometedora para la identificación, clasificación y pronóstico de la ERC.

Chronic kidney disease (CKD) high global prevalence, estimated between 11 to 13%, has been recognized as a mayor health challenge for healthcare systems due to its relevant economic and social implications. Main medical intervention strategies are directed to delay the progression of CKD and prevent outcomes. Serum creatinine concentration has been used to classify CKD and define its progression stage; however, it is well known the low sensitivity shown by this test. This fact has conducted to the search for new markers in order to improve the disease diagnosis, monitoring and treatment. In this context, metabolomics science and animal models have allowed identification of new metabolites that can be used as future biomarkers into clinical practice. This review aims to summarize the metabolomics profiles reported in different experimental models and clinical research on CKD. According with the data obtained, metabolites related with quaternary amines and aminoacid metabolic pathways like TMNO, indoxyl sulfate and dimethylarginine, suggest a promising alternative for identification, classification and prognosis of CKD.

Screening of Chemical Drugs in Fishery Inputs by Ultrahigh Performance Liquid Chromatography-Orbitrap High Resolution Mass spectroscopy / 分析化学

To screen the illegal substances in fishery inputs,we established the database including the precursor and the daughter ions for these possible components by the quadrupole/orbit-trap mass spectrometer,and the retention time of each drug on the same chromatographic column.And then,the extracted and diluted samples were analyzed and the components in the real samples were identified under the same conditions.Chromatographic analysis was performed on an Accucore RP-MS column (100 mm × 2.1 mm,2.6 μm) using gradient elution with 0.1％ formic acid in water and 0.1％ formic acid in acetonitrile as mobile phase.Elutes were ionized through heatable electrospray ionization (HESI) in both positive and negative mode simultaneously.Data acquisition was conducted by Full-scan ddMS2 (TopN) mode,in which the full mass profile for a continuous precursor ion injection and the fragments of each high abundant precursor of targeted were acquired with excellent time and mass resolution.Screening was carried out through comparison of the information of real samples with that of standards in the database,which were processed by software (Tracefinder).The Quantification of each component was analyzed based on the precursor ion chromatography acquired by orbit-trap mass spectroscopy,which showed a good linearity between 0.01-1 μg/mL,with R＞0.98.The method was validated by checking its minimum screening concentration (0.5 mg/L for drugs and 5 mg/L for feedstuffs) and evaluating the recovery after addition of the standard mixture in real samples (＞50％,under the addition of 10 and 100 mg/kg).The results for 68 practical samples demonstrated the effective performance of this method for screening with high-throughput,rapidness and acceptable minimum screening concentration and accuracy,in which 15 of 29 fishery drug samples were screened out for positive components that were not indicated in their labels.

Chemical composition, antioxidant and antibacterial activities of essential oil and methanol extract of Artemisia vulgaris and Gaultheria fragrantissima collected from Nepal

Objective To identify the chemical constituents and biological activities of essential oil and crude methanol extract of Artemisia vulgaris (A. vulgaris) and Gaultheria fragrantissima (G. fragrantissima). Methods Phytochemical screening, total phenolic and flavonoid content, antibacterial activities, anti-oxidant assay of the crude extract were carried out to identify the biological activities and phytonutrients present in the extract. Furthermore, the chemical constituents present in the essential oil and crude methanol extract were analyzed using gas chromatography mass spectroscopy and high performance liquid chromatography (HPLC) analysis. Results Gas chromatography mass spectroscopy analysis of essential oil from the aerial part of A. vulgaris revealed 24 different compounds in it. Sabinene (11.29%), β-thujone (19.19%), chrysanthenone (4.48%), camphor (11.89%), borneol (4.44%) and germacrene D (8.42%) were the major compounds. Similarly, leaves of G. fragrantissima contained methyl salicylate (95%) and asarone (4.64%). Furthermore, methanol extract of leaves of A. vulgaris and G. fragrantissima were found rich in the total flavonoids and phenolic content. HPLC analysis of the methanol extract of leaves A. vulgaris revealed the presence of morin and luteolin, whereas rutin was found as a major flavonoids compound in the leaves of G. fragrantissima. Further, methanol extract of the A. vulgaris and G. fragrantissima showed the highest antioxidant and antibacterial properties compared to the essential oil. Conclusions The HPLC analysis of the methanol extract of A. vulgaris shows the presence of luteolin and morin, whereas G. fragrantissima reveals the presence of rutin and a glycosylated flavonoids. Results reveal that A. vulgaris oil is the rich source of monoterpene and sesquiterpene compounds. Furthermore, A. vulgaris and G. fragrantissima are the rich source of the phenolic and flavonoids compounds and show good antioxidant and antibacterial activity.

Chemical composition, antioxidant and antibacterial activities of essential oil and methanol extract of Artemisia vulgaris and Gaultheria fragrantissima collected from Nepal

OBJECTIVE@#To identify the chemical constituents and biological activities of essential oil and crude methanol extract of Artemisia vulgaris (A. vulgaris) and Gaultheria fragrantissima (G. fragrantissima).@*METHODS@#Phytochemical screening, total phenolic and flavonoid content, antibacterial activities, anti-oxidant assay of the crude extract were carried out to identify the biological activities and phytonutrients present in the extract. Furthermore, the chemical constituents present in the essential oil and crude methanol extract were analyzed using gas chromatography mass spectroscopy and high performance liquid chromatography (HPLC) analysis.@*RESULTS@#Gas chromatography mass spectroscopy analysis of essential oil from the aerial part of A. vulgaris revealed 24 different compounds in it. Sabinene (11.29%), β-thujone (19.19%), chrysanthenone (4.48%), camphor (11.89%), borneol (4.44%) and germacrene D (8.42%) were the major compounds. Similarly, leaves of G. fragrantissima contained methyl salicylate (95%) and asarone (4.64%). Furthermore, methanol extract of leaves of A. vulgaris and G. fragrantissima were found rich in the total flavonoids and phenolic content. HPLC analysis of the methanol extract of leaves A. vulgaris revealed the presence of morin and luteolin, whereas rutin was found as a major flavonoids compound in the leaves of G. fragrantissima. Further, methanol extract of the A. vulgaris and G. fragrantissima showed the highest antioxidant and antibacterial properties compared to the essential oil.@*CONCLUSIONS@#The HPLC analysis of the methanol extract of A. vulgaris shows the presence of luteolin and morin, whereas G. fragrantissima reveals the presence of rutin and a glycosylated flavonoids. Results reveal that A. vulgaris oil is the rich source of monoterpene and sesquiterpene compounds. Furthermore, A. vulgaris and G. fragrantissima are the rich source of the phenolic and flavonoids compounds and show good antioxidant and antibacterial activity.

Simultaneous determination of ciprofloxacin hydrochloride and metronidazole in spiked human plasma by ultra performance liquid chromatography-tandem mass spectroscopy.

Ciprofloxacin HCl (CIP) and Metronidazole (MET) are antibacterial drugs used in combination for treatment of mixed aerobic/anaerobic infections. An UPLC-MS/MS method was developed for the simultaneous estimation of CIP and MET in spiked human plasma using sildenafil citrate as an internal standard (IS). Protein precipitation was used for analyte extraction. The chromatographic separation was completed within 6 min using a mobile phase of 0.1% formic acid in water and acetonitrile (70: 30, v/v), Zorbax C18, 100 x 4.6 mm, 3.5 μm analytical column, at a flow rate of 0.5 mL min-1. Multiple reaction monitoring (MRM) transitions were measured in the positive ion mode. Validation of the method showed standard curves to be linear in the range of 10-4000 ng mL-1 for CIP and 30-12000 ng mL-1 for MET with mean correlation coefficient exceeding 0.999. In human plasma, CIP and MET were stable for at least 36 days at –70 ± 5 °C, 6 hours at ambient temperature and after three freeze thaw cycles. After extraction from plasma, the samples were stable in auto sampler at 22 °C for 6 hours. The method was simple, specific, sensitive, precise, accurate and suitable for bioequivalence and pharmacokinetic studies.

Molecular Imaging for Theranostics in Gastroenterology: One Stone to Kill Two Birds

Molecular imaging in gastroenterology has become more feasible with recent advances in imaging technology, molecular genetics, and next-generation biochemistry, in addition to advances in endoscopic imaging techniques including magnified high-resolution endoscopy, narrow band imaging or autofluorescence imaging, flexible spectral imaging color enhancement, and confocal laser endomicroscopy. These developments have the potential to serve as "red flag" techniques enabling the earlier and accurate detection of mucosal abnormalities (such as precancerous lesions) beyond biomarkers, virtual histology of detected lesions, and molecular targeted therapy-the strategy of "one stone to kill two or three birds"; however, more effort should be done to be "blue ocean" benefit. This review deals with the introduction of Raman spectroscopy endoscopy, imaging mass spectroscopy, and nanomolecule development for theranostics. Imaging of molecular pathological changes in cells/tissues/organs might open the "royal road" to either convincing diagnosis of diseases that otherwise would only be detected in the advanced stages or novel therapeutic methods targeted to personalized medicine.

Proteomic and gene expression patterns of keratoconus.

Keratoconus is a progressive corneal thinning disease associated with significant tissue remodeling activities and activation of a variety of signaling networks. However, it is not understood how differential gene and protein expression direct function in keratoconus corneas to drive the underlying pathology, ectasia. Research in the field has focused on discovering differentially expressed genes and proteins and quantifying their levels and activities in keratoconus patient samples. In this study, both microarray analysis of total ribonucleic acid (RNA) and whole proteome analyses are carried out using corneal epithelium and tears from keratoconus patients and compared to healthy controls. A number of structural proteins, signaling molecules, cytokines, proteases, and enzymes have been found to be deregulated in keratoconus corneas. Together, the data provide clues to the complex process of corneal degradation which suggest novel ways to clinically diagnose and manage the disease. This review will focus on discussing these recent advances in the knowledge of keratoconus biology from a gene expression and function point-of-view.

Quantitative analysis of catechins in Saraca asoca and correlation with antimicrobial activity / 药物分析学报

Herbal medicines are highly complex and have unknown mechanisms in diseases treatment. Saraca asoca (Roxb.), De. Wild has been recommended to treat gynecological disorders and used in several commercial polyherbal formulations. In present study, efforts have been made to explore antimicrobial activity and its co-relation with the distributions of catechins in the organs of S. asoca using targeted MS/MS. Eight extracts (cold and hot water) from four different organs of S. asoca and two drugs were prepared and antimicrobial activity was assessed by microbroth dilution assay. Quantitative and qualitative analysis of catechins in crude extracts was done by using targeted and auto-MS/MS and correlated with antimicrobial activity. (t)-Catechin and (t)-epicatechin and their biosynthesis related compound were found to be up-regulated in regenerated bark and leaves extracts. (?)-Epigallocatechin was found to be significantly higher in bark water extract as compared to others but showed low antimicrobial activity. Result showed down-regulation of (?)-epigallocatechin and up-regulation of (t)-catechin and (t)-epicatechin in the regenerated bark and leaves of S. asoca. It might be the contributing factor in the antimicrobial activity of regenerated bark and leaves of the plant. The concentration of (t)-epicatechin in processed drugs (Ashokarishta) from Baidyanath was found to be seven times higher than that of Dabur Pvt. Ltd., but no antimicrobial activity was observed, indicating the variations among the plant based drugs. This will be helpful in rational use of S. asoca parts. Furthermore, the analytical method developed is sensitive, repeatable and reliable; therefore, it is suitable for quality control of herbal drugs.

Biological Effect of Heavy Metal in Drinking Water samples of Western Uttar Pradesh region in India.

Drinking water is a basic requirement for life and a determinant of standard of living. Poor water quality problem has also been observed in more number of habitations. Drinking water, in adequate quantity with safe quality is a basic requirement for life and a determinant of standard of living. Certain health problems are associated with people due to presence of excess of heavy metals and other impurities. The present study was conducted to analyze the various parameters of ground water in Uttar Pradesh India and to check its fitness for drinking. It will also clarify the health hazards imposed on the population of this state. The water samples are collected from Aligarh, Bulandshar, Merrut, MuzaffarNagar & Saharanpur zone of the Western U.P. region. Ten samples of ground water were collected from each of the five regions during the pre-mansoon (Jan-Feb) and post-mansoon (Sept-Oct ) seasons. The pH was estimated by pH meter, acidity, alkalinity, sulphates, chorides, Total hardness(Ca & Mg) were determined by titration methods. The total suspended solid was calculated by the formula. The heavy metals like Mn, Al, Ba, Cd, Cr, Co, Cu, Fe and Pb were determined in the ground water samples by ICP mass spectroscopy. The concentrations of heavy metals, pH, alkalinity, sulphate, chloride, TDS & Total Hardness (TH) were compared with the standards by BIS for Drinking water (IS 10500:2004). The results shows that water pH of all the five regions showed no remarkable variation from the BIS recommended value of pH (6.5-8.5). The alkalinity was above the BIS desirable level of 200mg/l in all the samples, but was less than the maximum permissible limit. The Drinking water of all the regions contains higher amounts of TDS than the desirable limits. Maximum TDS was detected in aligarh(780-820mg/litre). The ground water of Saharanpur region shows total hardness to be above the BIS desirable level of 300mg/l. The chloride content was above the BIS desirable level of 250mg/l in Aligarh only. The sulphate content was highest in aligarh (223mg/l). The Cd, Cr, &Pb content of all the five regions of Uttar Pradesh showed higher the BIS permissible limits of 0.003, 0.05 and 0.01mg/l respectively. The content of Mn, Ba, Cu, Co & Fe are within the permissible limit of BIS standards for drinking water.

Isolation and charecterization of an antimicrobial protein from the liver of goat (capra hircus)

Antimicrobial proteins (AMPs) have become recognized as important components of the non specific host defense or innate system in a variety of organisms including bacteria, fungi, plants, insects, birds, amphibians, mammals and crustaceans. In the present study an AMP was isolated from the liver of CAPRA HIRCUS (Goat). Protein was isolated from the freshly collected liver tissue. Further acidic, basic and neutral fractions of protein were obtained and their antimicrobial activity was checked against B. Subtilis, E. Coli, P. Vulgaris and Enterobacter. The protein fractions having antimicrobial activity was subjected to SDS PAGE. The separated fractions were further processed for mass spectroscopy (LCQ-Fleet Mass Spectrophotometer) and their mass was deduced by the spectral data analysis. The amino acid sequence (FGGGMA) was deduced from the peaks obtained in mass spectroscopy which was having mass of 0.8 KD.

Analytical study of water safety parameters in ground water samples of Uttarakhand in India.

The main problem of the locality is the drinking water. Certain health problems are associated with people living in hills that are because of the presence of excess of heavy metals and other impurities. The present study was conducted to analyze the various parameters of ground water in uttarakhand, India and to check its fitness for drinking. It will also clarify the health hazards imposed on the population of this state. The present study was conducted in five regions of Uttarakhand, India (Haridwar, Vikasnagar, Mussoorie, Dehradun & Dakpathar). Ten samples of ground water were collected from each of the five regions during the pre-mansoon (Jan-Feb ) and post-mansoon (Sept-Oct )seasons.The pH was estimated by pH meter, acidity,alkalinity, sulphates,chorides,Total hardness(Ca & Mg) were determined by titration methods. The total suspended solid was calculated by the formula. The heavy metals like Mn, Al, Ba, Cd, Cr, Co, Cu, Fe and Pb were determined in the ground water samples by ICP mass spectroscopy. The concentrations of heavy metals, pH, alkalinity, sulphate, chloride, TDS & Total Hardness (TH) were compared with the standards by BIS for Drinking water (IS 10500:1991). The results shows that water pH of all the five regions showed no remarkable variation from the BIS recommended value of pH (6.5-8.5). The alkalinity was above the BIS desirable level of 200mg/l in all the samples, but was less than the maximum permissible limit. The Drinking water of all the regions contains higher amounts of TDS than the desirable limits. maximum TDS was detected in Haridwar & dehradun state. The ground water of mussoorie region shows total hardness to be above the BIS desirable level of 300mg/l. The chloride content was above the BIS desirable level of 250mg/l in dehradun only. The sulphate content was highest in haridwar (197.5mg/l) and dehradun (170mg/l) but it was below the desirable limit of 200mg/l. The Cd,Cr,&Pb content of all the five regions of Uttarakhand showed higher the BIS permissible limits of 0.01, 0.05 and 0.05 mg/l respectively. The content of Mn,Ba,Cu, Co&Fe are within the permissible limit of BIS standards for drinking water.

In vivo pharmacokinetics of salvianolic acid B and its metabolite in rats / 中草药

Objective: A rapid and sensitive method using liquid chromatography-tandem mass spectroscopy (LC-MS/MS) was developed and validated for the simultaneous quantitative determination of salvianolic acid B (Sal B) and its main active metabolite danshensu(DSS) in rat plasma. Methods: The analytes were extracted by liquid-liquid extraction with ethyl acetate after IS (IS, chloramphenicol) spiked. The separation was performed on a Symmetry C18 column with methanol-acetonitrile-0.5% formic acid (55:5:40) as mobile phase at a flowrate of 0.4 mL/min. The triple quadrupole LC-MS system was operated under selected reaction monitoring (SRM) mode using the electrospray ionization technique in negative mode. Quantification was performed using SRM of the transitions m/z 717→519 for Sal B, 197→135 for DSS, and 321→152 for the IS, respectively. Results: The nominal retention times for Sal B, DSS , and IS were 3.12, 2.60, and 3.98 min, respectively. The standard calibration curve for spiked rat plasma containing Sal B was linear over the range 10-5 000 ng/mL with a correlation coefficient (r >0.995). And DSS was linear over the range 5-5000 ng/mL with a correlation coefficient (r>0.995). The lower limits of quantification (LLOQ) of Sal B and DSS of the method were 10 and 5 ng/mL, respectively. The intra- and inter-day accuracy and precision of the assay were less than 12.6%. After Sal B was ig administered to rats, absorption of Sal B was rapidly metabolized to DSS. Pharmacokinetic parameters of Sal B and DSS after ig administration Sal B to Wistar rats were: Cmax (1.21±0.31) and (0.27±0.05) μg/mL, tmax (0.50±0.00) and (0.56±0.18) h, t1/2 (1.20±0.11) and (1.57±0.16) h, AUC0-1 (1.31±0.30) and (0.39±0.05) μg·mL-1·h. Conclusion: This method has been applied successfully to a pharmacokinetic study of Sal B and its metabolite DSS involving the ig administration of Sal B to rats.

Structure elucidation of a flavonoid glycoside from the roots of Clerodendrum serratum (L.) Moon, Lamiaceae

Apigenin-7-glucoside, C21H20O10 (7-(β-D-glucopyranosyloxy)-5-hydroxy-2-(4-hydroxyphenyl)-4H-1-benzopyran-4-one), was first time isolated from the roots of Clerodendrum serratum (L.) Moon, Lamiaceae. Structure elucidation of the compound was carried out by ¹H NMR and FAB-MS studies.

Apigenin-7-glucosídeo, C21H20O10 (7-(β-D-glucopiranosiloxi)-5-hidroxi-2-(4-hidroxifenil)-4H-1-benzopiran-4-ona), foi isolado pela primeira vez das raízes de Clerodendrum serratum (L.) Moon, Lamiaceae. A elucidação estrutural da susbtância foi feita através de estudos de ¹H NMR e FAB-MS.

Simultaneous detection of strychnine and brucine in biological matrix by gas chromatography-mass spectroscopy.

A new gas chromatography-mass spectroscopy (GC-MS) method is being presented for the separation and detection of strychnine and brucine, alkaloids of Strychnos nux vomica in a single run. The analysis was carried out using 5% phenyl methyl silicone capillary column, electron impact ionization mode and quadrupole mass analyzer. The extracts of the exhibits were analyzed using the new method. The peaks of the two alkaloids were found to be well resolved, and there was clear separation between the two. The retention time and mass fragmentation pattern, base peaks, molecular peaks of strychnine and brucine standard/NIST library and crime case exhibits matched, establishing the presence of the two active principles of Strychnos nux vomica. The new method has the advantage of better separation of the two alkaloid peaks over the conventional GC-MS methods, and is useful for the identification and confirmation of Strychnos nux vomica constituents in biological matrices of poisoning cases that have ended in death.

Mass spectroscopy investigation of the effect of gamma irradiation on the mean value of the number of ethoxy groups in the triton x-100 / Estudio del efecto de la radiación gamma en elvalor medio del número de grupos etoxiLados del surfactante Tritón X-100

El efecto de la radiación gamma proveniente de una fuente de 60Co en la estructura del surfactante no iónico Tritón X-100 fue investigado. Tres regiones principales pueden ser distinguidas en el comportamiento del valor medio del número de grupos etóxidos al aumentar la dosis. Sin embargo, el resultado global encontrado fue una pequeña variación en este valor medio al cambiar la dosis entre 0 y 70 KGy.

The effect of gamma radiation from a 60Co source on the structure of a nonionic surfactant, namely TRITON X-100, was investigated. Three main regions can be distinguished in the behavior of the mean value of ethoxy groups with an increase in the absorbed dose. However just a slightly decrease on this mean value was obtained when the dose range from 0 to 70 kGy.

Rapid Screening Method for Ten Sedative-hypnotica Drug in Functional Food by Liquid Chromatography with Mass Spectrometry / 环境与健康杂志

Objective To develop a method for the simultaneous separation and determination of 10 kinds of sedative hypnotica drugs in the functional food with high performance liquid chromatography mass spectrometry system.Methods The mobile phase consisted of acetonitrile and 15 mmol/L ammonium acetate solution(0.1% formic acid ),chromatographic column was Zobax SB C 18.Identification was based on the compound's absolute retention time,protonated molecular ion,and representative fragment ion by multiple reaction monitoring.The condition of determination was investigated and optimized.Results With this method,the linear range for the 10 drugs was 10-1 080 ?g/kg,the average recoveries ranged from 80.5%-97.1% and the detection limits were from 0.35-12.0?g/kg respectively.Conclusion The method established in the present paper is applicable to monitoring sedative hypnotica drug in the functional food.