ABSTRACT
The diverse tea (Camellia sinensis) germplasms in China include those that specifically accumulate metabolites, such as anthocyanin, catechin, amino acid, caffeine, aroma compound, and chlorophyll. There is interest in the derived products because of special flavor quality or high efficacy activity. This review describes the characteristics of specific tea germplasms and associated regulatory mechanisms. High expression levels of the corresponding biosynthetic genes lead to the substantial accumulation of anthocyanins. The increased metabolic flux from anthocyanins to galloylated catechins is responsible for the occurrence of high-catechin germplasms. The precursor ethylamine determines the differential abundance of l-theanine between tea and other plants. The high amino acid contents in albino germplasms are the result of decreased l-theanine hydrolysis. In low-caffeine tea germplasms, caffeine synthase genes are minimally expressed or mutated. High-aroma germplasms are associated with an increase in the precursors or strong stress-induced responses. Enhanced chloroplast and chlorophyll synthesis is a hallmark of the high-chlorophyll germplasms. Overall, biosynthetic metabolism might have contributed to the occurrence of specific tea germplasms. Furthermore, elucidation the deeper molecular mechanisms in specific tea germplasms are significant and urgent. The information will enhance our understanding of the metabolic activities in tea plants, with implications for tea breeding.
Subject(s)
Camellia sinensis , Catechin , Anthocyanins/analysis , Caffeine/analysis , Camellia sinensis/chemistry , Catechin/analysis , Chlorophyll/analysis , Ethylamines/analysis , Ethylamines/metabolism , Plant Breeding , Plant Leaves/chemistry , Tea/metabolismABSTRACT
The production and consumption of new psychoactive substances (NPSs) has been raising a major concern worldwide. Due to easy access and available information, many NPSs continue to be synthesized with an alarming increase of those available to purchase, despite all the control efforts created. A new analytical method was developed and validated to determine a group of phenethylamines and synthetic cathinones: cathinone, flephedrone, buphedrone, 4-MTA, α-PVP, methylone, 2C-P, ethylone, pentylone, MDPV and bromo-dragonFLY in whole blood. A mixed-mode solid phase extraction was applied to 250 µL of sample, and the extracts were derivatized with fast microwave technique before being analyzed by gas chromatography-mass spectrometry (GC-MS). The validation procedure followed the Scientific Working Group for Forensic Toxicology (SWGTOX) guidelines with parameters that included selectivity, linearity, limits of detection and quantification, intra- and inter-day precision and accuracy, recoveries and stability. The method presented linearity between 5 and 500 ng/mL for cathinone, buphedrone, 4-MTA, methylone, 2C-P and bromo-dragonFLY, 10-500 ng/mL for flephedrone, ethylone, pentylone and MDPV, and 40-500 ng/mL for α-PVP, with determination coefficients above 0.99 for all analytes. Recoveries ranged between 70.3% and 116.6%, and regarding intra- and inter-day precision, the relative mean errors were typically lower than 8.6%. The method was successfully applied to over 100 authentic samples from the Laboratory of Chemistry and Forensic Toxicology, Centre Branch, of the National Institute of Legal Medicine and Forensic Sciences, Portugal.
Subject(s)
Designer Drugs/metabolism , Forensic Toxicology , Microwaves , Psychotropic Drugs/blood , Substance Abuse Detection/methods , Acetone/analogs & derivatives , Acetone/analysis , Acetone/blood , Alkaloids/analysis , Alkaloids/blood , Amphetamines/analysis , Amphetamines/blood , Designer Drugs/analysis , Ethylamines/analysis , Ethylamines/blood , Gas Chromatography-Mass Spectrometry , Humans , Limit of Detection , Methamphetamine/analogs & derivatives , Methamphetamine/analysis , Methamphetamine/blood , Pentanones/analysis , Pentanones/blood , Phenethylamines/analysis , Phenethylamines/blood , Pyrrolidines/analysis , Pyrrolidines/bloodABSTRACT
l-Theanine is a specialized metabolite in tea (Camellia sinensis) leaves that contributes to tea function and quality. Yellow tea leaves (albino) generally have higher l-theanine contents than green tea leaves (normal), but the reason is unknown. The objective of this study was to investigate why l-theanine is accumulated in yellow tea leaves. We compared original normal leaves (green) and light-sensitive albino leaves (yellow) of cv. Yinghong No. 9. The l-theanine content was significantly higher in yellow leaves than in green leaves (pâ¯≤â¯0.01). After supplementation with [2H5]-l-theanine, yellow leaves catabolized less [2H5]-l-theanine than green leaves (pâ¯≤â¯0.05). Furthermore, most plants contained the enzyme catalyzing l-theanine conversion to ethylamine and l-glutamic acid. In conclusion, l-theanine accumulation in albino-induced yellow tea leaves was due to weak l-theanine catabolism. The differential accumulation mechanism differed from the l-theanine accumulation mechanism in tea and other plants.
Subject(s)
Camellia sinensis/chemistry , Glutamates/analysis , Plant Leaves/chemistry , Camellia sinensis/metabolism , Ethylamines/analysis , Ethylamines/metabolism , Glutamates/metabolism , Glutamic Acid/analysis , Glutamic Acid/metabolism , Hydrolases/metabolism , Plant Leaves/metabolismABSTRACT
An improved ion chromatographic method including two elution procedures was proposed for the quantitative determination of atmospheric alkylamines in field atmospheric samples involving high levels of inorganic cations by using 18-crown-6 as mobile phase additive. When 18-crown-6 was added to the mobile phase, the retention times increased significantly for Na+, NH4+, K+ and primary alkylamines but decreased for secondary and tertiary alkylamines due to the complexation with certain cations and interaction with both stationary and mobile phases of 18-crown-6. As a result, the separation of the cations was greatly promoted, which reduced the interference of peak distortion of overloaded inorganic cations on the quantitation of adjacent alkylamines. By using the presented method, five inorganic cations (Na+, NH4+, K+, Mg2+, Ca2+) and six alkylamines (dimethylamine (DMAH+), trimethylamineâ¯+â¯diethylamine (TMAH+â¯+â¯DEAH+), propylamine (MPAH+), triethylamine (TEAH+), ethanolamine (MEOAH+) and triethanolamine (TEOAH+)) were effectively separated and determined, and the relative standard derivations (RSDs) of objective cations were all less than 1% for retention time and 3.1% for peak area (nâ¯=â¯9), respectively. The linearity was excellent for each cation (R2â¯>â¯0.993) except for NH4+ and TEOAH+ showing a non-linear response (R2â¯>â¯0.998 for theoretical non-linear fitting), and the detection limit of these cations were 0.03-1.19â¯ng. The proposed method was successfully used in the determination of both alkylamines and inorganic cations in ambient particulate matters and gaseous alkylamines in ceiling duct exhaust. The annual average concentrations of DMAH+, TMAH+â¯+â¯DEAH+ and TEAH+ were 15.56, 4.35 and 16.00â¯ngâ¯m-3 in PM2.5 over Shanghai in 2013. The concentrations of gaseous DMA and TMAâ¯+â¯DEA in ceiling duct exhaust reached a maximum of 940.0 and 112.7⯵gâ¯m-3, and were positively correlated with the human activity intensity, suggesting that human excreta emissions was a potential important source of atmospheric alkylamines in urban area of Shanghai.
Subject(s)
Chromatography, Ion Exchange/methods , Crown Ethers/chemistry , Ethylamines/analysis , Methylamines/analysis , Air Pollutants/analysis , Cations/chemistry , Gases/chemistry , Humans , Particulate Matter/analysisABSTRACT
Application of HIV-1 protease inhibitors (as an anti-HIV regimen) may serve as an attractive strategy for anti-HIV drug development. Several investigations suggest that there is a crucial need to develop a novel protease inhibitor with higher potency and reduced toxicity. Monte Carlo optimized QSAR study was performed on 200 hydroxyethylamine derivatives with antiprotease activity. Twenty-one QSAR models with good statistical qualities were developed from three different splits with various combinations of SMILES and GRAPH based descriptors. The best models from different splits were selected on the basis of statistically validated characteristics of the test set and have the following statistical parameters: r2 = 0.806, Q2 = 0.788 (split 1); r2 = 0.842, Q2 = 0.826 (split 2); r2 = 0.774, Q2 = 0.755 (split 3). The structural attributes obtained from the best models were analysed to understand the structural requirements of the selected series for HIV-1 protease inhibitory activity. On the basis of obtained structural attributes, 11 new compounds were designed, out of which five compounds were found to have better activity than the best active compound in the series.
Subject(s)
Drug Discovery , Ethylamines/chemistry , HIV Protease Inhibitors/chemistry , Quantitative Structure-Activity Relationship , Ethylamines/analysis , HIV Protease Inhibitors/analysis , Models, Molecular , Monte Carlo MethodABSTRACT
BACKGROUND: Foundry workers are occupationally exposed to hazardous substances such as silica dusts and toxic gases. The aim of this study was to examine the effects of simultaneous exposure to complex mixtures of silica dust, formaldehyde, and triethylamine on lung function parameters. STUDY DESIGN: A cross-sectional study. METHODS: This study was conducted on 55 male workers of core making unit of a foundry plant (the case group) and 55 workers in a food industry were enrolled as a control group in 2015. Workers were monitored for personal exposure to crystalline silica respirable dust, according the NIOSH method No.7602. The concentrations of formaldehyde and triethylamine were measured using a PID instrument. Lung function tests were performed according to the ERS/ATS standards. RESULTS: The mean concentrations of personal exposure to silica dust, formaldehyde, and triethylamine in the core making workers were 0.23 mg/m3, 2.85 ppm, and 5.55 ppm and respective exposures of control subjects were less than the LOD (limit of detection). There were significant associations between exposure to silica dust and decreases in FVC (Forced vital capacity) values (P<0.05). The findings showed a statistically significant synergistic effect of silica dust and triethylamine on FVC values (P<0.05). CONCLUSIONS: The mean exposure of all studied substances was higher than occupational exposure limits. Synergistic effects of exposure to silica dust and triethylamine on some lung function parameters were observed. Simultaneous exposure of foundry workers to silica dust and triethylamine could impair lung function.
Subject(s)
Air Pollutants/adverse effects , Ethylamines/adverse effects , Formaldehyde/adverse effects , Lung/drug effects , Manufacturing Industry , Occupational Exposure/adverse effects , Silicon Dioxide/adverse effects , Adult , Air Pollutants/analysis , Complex Mixtures/adverse effects , Cross-Sectional Studies , Dust/analysis , Environmental Monitoring/methods , Ethylamines/analysis , Formaldehyde/analysis , Humans , Lung/physiology , Male , Occupational Exposure/analysis , Occupations , Respiratory Function Tests , Silicon Dioxide/analysis , Vital Capacity , WorkABSTRACT
In this study, a novel solid phase microextration (SPME) Arrow was prepared for the sampling of volatile low molecular weight alkylamines (trimethylamine (TMA) and triethylamine (TEA)) in wastewater, salmon and mushroom samples before gas chromatographic separation with mass spectrometer as detector. Acidified zeolitic imidazolate framework-8 (A-ZIF-8) was utilized as adsorbent and poly(vinyl chloride) (PVC) as the adhesive. The custom SPME Arrow was fabricated via a physical adhesion: (1) ZIF-8 particles were suspended in a mixture of tetrahydrofuran (THF) and PVC to form a homogeneous suspension, (2) a non-coated stainless steel SPME Arrow was dipped in the ZIF-8/PVC suspension for several times to obtain a uniform and thick coating, (3) the pore size of ZIF-8 was modified by headspace exposure to hydrochloric acid in order to increase the extraction efficiency for amines. The effect of ZIF-8 concentration in PVC solution, dipping cycles and aging temperature on extraction efficiency was investigated. In addition, sampling parameters such as NaCl concentration, sample volume, extraction time, potassium hydroxide concentration, desorption temperature and desorption time were optimized. The Arrow-to-Arrow reproducibilities (RSDs) for five ZIF-8 coated Arrows were 15.6% and 13.3% for TMA and TEA, respectively. The extraction with A-ZIF-8/PVC Arrow was highly reproducible for at least 130 cycles without noticeable decrease of performance (RSD<12.5%). Headspace SPME of 7.5mL sample solution with the fabricated ZIF-8 coated Arrow achieved linear ranges of 1-200ngmL-1 for both TMA and TEA. The limit of quantitation (LOQ) was 1ngmL-1 for both TMA and TEA. The method was successfully applied to the determination of TMA and TEA in wastewater, salmon and mushroom samples giving satisfactory selectivity towards the studied amines.
Subject(s)
Amines/analysis , Amines/chemistry , Food Analysis/methods , Gas Chromatography-Mass Spectrometry , Imidazoles/chemistry , Solid Phase Microextraction/methods , Wastewater/chemistry , Zeolites/chemistry , Agaricales/chemistry , Animals , Ethylamines/analysis , Ethylamines/chemistry , Methylamines/analysis , Methylamines/chemistry , Molecular Weight , Polyvinyl Chloride/chemistry , Salmon , Seafood , Sodium Chloride/chemistry , Solid Phase Microextraction/instrumentation , Stainless Steel/chemistry , TemperatureABSTRACT
The drinking water sources of many cities in southern China are frequently contaminated by upstream urban drainage during storm events, which brings high concentrations of N-nitrosamine (NA) precursors and poses a threat to the safety of drinking water. We conducted two sampling campaigns during the heavy rain season in 2015 in one representative city in southern China. We detected that the concentration of N-nitrosodimethylamine formation potential (NDMA FP) in urban drainage during two storm events was 80-115 ng/L and the total formation potential concentration of nine nitrosamines (TNA9 FP) was 145-165 ng/L. To address the deteriorated water quality, 30 mg/L of powdered activated carbon (PAC) was fed into the water intake. PAC adsorption alone could remove 52% of NDMA FP and 52% of TNA FP, while the subsequent conventional process only removed 8% of TNA FP. We isolated six chemicals (N,N-benzyldimethylamine, 5-[(dimethylamino)methyl]-2-furanmethanol, N,N-dimethyl-3-aminophenol, N,N-dimethylethylamine, Ziram, and N,N-dimethylaniline) and confirmed them to be NA precursors. Among these NA precursors, Ziram was identified for the first time as a NA precursor that is formed via chloramination; its molar yield for NDMA was 6.73 ± 0.40%.
Subject(s)
Drainage, Sanitary , Drinking Water/analysis , Nitrosamines/analysis , Rain , Water Pollutants, Chemical/analysis , Water Purification/methods , Adsorption , Aniline Compounds/analysis , Charcoal/chemistry , China , Cities , Dimethylnitrosamine/analysis , Disinfection , Ethylamines/analysis , Water QualityABSTRACT
Skin powders and aqueous alcohol extracts were obtained from waste marcs from different grape varieties (Barbera, Nebbiolo, Pinot Noir, Chardonnay, Moscato and Müller-Thurgau). Both skins and extracts were analysed for the content of chemical contaminants: ochratoxin A (OTA), biogenic amines (BIAs), pesticides and metals. OTA was detected in low concentrations in Barbera, Moscato and Nebbiolo skins, but only in Barbera and Moscato extracts. Cadaverine, putrescine, ethanolamine and ethylamine were found in extracts at very low levels, while potential allergenic amines, tyramine and histamine, were never detected. Different pesticides were present in both skins and extracts. Pb and Cd were found in trace only in the powders, and K, Ca and Mg were the most abundant elements in both skin powders and extracts. Concentrations of the different contaminants were related to fibre content or total phenolics content of powders and extracts, respectively, in order to evaluate their use in the food sector.
Subject(s)
Food Safety , Fruit/chemistry , Vitis/chemistry , Waste Products/analysis , Biogenic Amines/analysis , Cadaverine/analysis , Calcium/analysis , Chromatography, High Pressure Liquid , Ethanolamine/analysis , Ethylamines/analysis , Humans , Liquid-Liquid Extraction/methods , Magnesium/analysis , Ochratoxins/analysis , Pesticides/analysis , Potassium/analysis , Powders , Putrescine/analysisABSTRACT
A 30-year-old man reportedly ingested pills and used illicit drugs with another person. They both fell asleep that night and the following afternoon the other person found him dead. There were used hypodermic needles and a metal spoon with dark tarry substance at the death scene, and two recent puncture sites were found on his body. It was uncertain if he had a history of illicit drug use. Postmortem blood initially screened borderline positive for methamphetamine by ELISA. An alkaline drug screen-detected ethylone which was subsequently confirmed and quantified by a specific GC-MS SIM analysis following solid-phase extraction. Concentrations were determined in the peripheral blood (0.39 mg/L), central blood (0.38 mg/L), liver (1.4 mg/kg), vitreous (0.58 mg/L), urine (20 mg/L) and gastric contents (12 mg). Other compounds detected in peripheral blood were morphine (0.05 mg/L), alprazolam (<0.05 mg/L), delta-9-THC (<1 ng/mL), delta-9-carboxy-THC (3.6 ng/mL) and naproxen (<5 mg/L). A urine screen (GC-MS) also confirmed 6-monoacetylmorphine, codeine and sildenafil. The cause of death was certified due to mixed ethylone, heroin and alprazolam intoxication. The manner of death was certified as accident.
Subject(s)
Acetone/analogs & derivatives , Drug Overdose/diagnosis , Ethylamines/poisoning , Illicit Drugs/poisoning , Substance-Related Disorders/diagnosis , Accidents , Acetone/analysis , Acetone/poisoning , Adult , Alprazolam/analysis , Autopsy , Cause of Death , Drug Overdose/metabolism , Enzyme-Linked Immunosorbent Assay , Ethylamines/analysis , Fatal Outcome , Forensic Toxicology/methods , Gas Chromatography-Mass Spectrometry , Heroin/analysis , Humans , Illicit Drugs/analysis , Male , Predictive Value of Tests , Solid Phase Extraction , Substance Abuse Detection/methods , Substance-Related Disorders/metabolismABSTRACT
Alkylamines are associated with both natural and anthropogenic sources and have been detected in ambient aerosol in a variety of environments. However, little is known about the ubiquity or relative abundance of these species in Europe. In this work, ambient single-particle mass spectra collected at five sampling sites across Europe have been analysed for their alkylamine content. The aerosol time-of-flight mass spectrometer (ATOFMS) data used were collected in Ireland (Cork), France (Paris, Dunkirk and Corsica) and Switzerland (Zurich) between 2008 and 2013. Each dataset was queried for mass spectral marker ions associated with the following ambient alkylamines: dimethylamine (DMA), trimethylamine (TMA), diethylamine (DEA), triethylamine (TEA), dipropylamine (DPA) and tripropylamine (TPA). The fraction of ambient particles that contained detectable alkylamines ranged from 1 to 17 % depending on location, with the highest fractions observed in Paris and Zurich in the winter months. The lowest fractions were observed at coastal sites, where the influence of animal husbandry-related alkylamine emissions is also expected to be lowest. TMA was the most ubiquitous particle phase alkylamine detected and was observed at all locations. Alkylamines were found to be internally mixed with both sulphate and nitrate for each dataset, suggesting that aminium salt formation may be important at all sites investigated. Interestingly, in Corsica, all alkylamine particles detected were also found to be internally mixed with methanesulphonic acid (MSA), indicating that aminium methanesulphonate salts may represent a component of marine ambient aerosol in the summer months. Internal mixing of alkylamines with sea salt was not observed, however. Alkylamine-containing particle composition was found to be reasonably homogeneous at each location, with the exception of the Corsica and Dunkirk sites, where two and four distinct mixing states were observed, respectively.
Subject(s)
Aerosols/analysis , Air Pollutants/analysis , Diethylamines/analysis , Dimethylamines/analysis , Ethylamines/analysis , Methylamines/analysis , Propylamines/analysis , Cities , Environmental Monitoring/methods , Europe , Mass Spectrometry/methods , Particle Size , Seasons , Sulfates/analysisABSTRACT
Mechanical abrasion is an extremely simple, rapid, and low-cost method for deposition of carbon-based materials onto a substrate. However, the method is limited in throughput, precision, and surface compatibility for drawing conductive pathways. Selective patterning of surfaces using laser-etching can facilitate substantial improvements to address these current limitations for the abrasive deposition of carbon-based materials. This study demonstrates the successful on-demand fabrication of fully-drawn chemical sensors on a wide variety of substrates (e.g., weighing paper, polymethyl methacrylate, silicon, and adhesive tape) using single-walled carbon nanotubes (SWCNTs) as sensing materials and graphite as electrodes. Mechanical mixing of SWCNTs with solid or liquid selectors yields sensors that can detect and discriminate parts-per-million (ppm) quantities of various nitrogen-containing vapors (pyridine, aniline, triethylamine).
Subject(s)
Aluminum Oxide/chemistry , Carbon/chemistry , Paper , Polymethyl Methacrylate/chemistry , Silicon/chemistry , Aniline Compounds/analysis , Electrodes , Ethylamines/analysis , Glass/chemistry , Pyridines/analysis , Surface PropertiesABSTRACT
The branching ratios for the reaction of the OH radical with the primary and secondary alkylamines: methylamine (MA), dimethylamine (DMA), and ethylamine (EA), have been determined using the technique of pulsed laser photolysis-laser-induced fluorescence. Titration of the carbon-centered radical, formed following the initial OH abstraction, with oxygen to give HO2 and an imine, followed by conversion of HO2 to OH by reaction with NO, resulted in biexponential OH decay traces on a millisecond time scale. Analysis of the biexponential curves gave the HO2 yield, which equaled the branching ratio for abstraction at αC-H position, r(αC-H). The technique was validated by reproducing known branching ratios for OH abstraction for methanol and ethanol. For the amines studied in this work (all at 298 K): r(αC-H,MA) = 0.76 ± 0.08, r(αC-H,DMA) = 0.59 ± 0.07, and r(αC-H,EA) = 0.49 ± 0.06 where the errors are a combination in quadrature of statistical errors at the 2σ level and an estimated 10% systematic error. The branching ratios r(αC-H) for OH reacting with (CH3)2NH and CH3CH2NH2 are in agreement with those obtained for the OD reaction with (CH3)2ND (d-DMA) and CH3CH2ND2 (d-EA): r(αC-H,d-DMA) = 0.71 ± 0.12 and r(αC-H,d-EA) = 0.54 ± 0.07. A master equation analysis (using the MESMER package) based on potential energy surfaces from G4 theory was used to demonstrate that the experimental determinations are unaffected by formation of stabilized peroxy radicals and to estimate atmospheric pressure yields. The branching ratio for imine formation through the reaction of O2 with α carbon-centered radicals at 1 atm of N2 are estimated as r(CH2NH2) = 0.79 ± 0.15, r(CH2NHCH3) = 0.72 ± 0.19, and r(CH3CHNH2) = 0.50 ± 0.18. The implications of this work on the potential formation of nitrosamines and nitramines are briefly discussed.
Subject(s)
Dimethylamines/analysis , Ethylamines/analysis , Hydroxyl Radical/chemistry , Methylamines/analysis , Atmosphere , Ethanol/analysis , Kinetics , Methanol/analysis , Nitric Oxide/chemistry , Reproducibility of ResultsABSTRACT
A direct injection gas chromatography method was developed for the determination of triethylamine and dimethyl sulfoxide (DMSO) in a drug substance (ML-189). Matrix effects were found to result in the overestimation of DMSO when methanol was used as diluent. Multiple approaches to eliminate matrix effects were unsuccessful; these included changes in sample size, split ratio, injector temperature and injector liner (e.g., deactivated liner). Ultimately, matrix effects were eliminated after the diluent was changed from methanol to acetone. A mechanism was proposed and discussed.
Subject(s)
Chromatography, Gas/methods , Dimethyl Sulfoxide/analysis , Ethylamines/analysis , Chemistry, Pharmaceutical , Linear Models , Pharmaceutical Preparations/chemistry , Reproducibility of Results , Sensitivity and SpecificityABSTRACT
We have recently reported a novel class of selective 5-HT1A agonists among which GF449 emerged for its high potency and almost full agonist activity (pKi 5-HT1A = 8.8; pD2 = 9.22, %Emax = 91.6). In order to quantify GF449 in rat plasma and brain, a sensitive LC-MS/MS method was developed and validated. Solid phase extraction (SPE) or a combined protein precipitation SPE permitted an efficient analyte recovery and sample clean-up. Multiple reaction monitoring (MRM) was used to track both GF449 and its internal standard (IS), MM189. GF449 was determined and quantitated to nanomolar concentrations in both plasma and brain matrix (LOQs = 0.0025 nmol/mL). Specificity was ensured using three further MRM qualifier transitions for both analyte and IS. Linearity was found in the range of 0.0025 nmol/mL to 1.00 nmol/mL (R(2) = 0.9965) and from 0.0025 nmol/mL to 50 nmol/mL (R(2) = 0.9999) for plasma and brain respectively. Intraday trueness ranged from 94.0% to 117.5% for brain and from 93.7% to 108.1% for plasma, while precision values were within 3.0% - 6.7% and 2.5% - 9.2% for plasma and brain respectively. The interday trueness of plasma ranged from 89.6% to 107.7% and the precision values (CV%) ranged from 4.6% to 7.5%. Interday trueness and precision (CV%) of the brain ranged from 94.3% to 101.2% and from 1.6% to 11.5% respectively. The method was validated in accordance with the EMEA guidelines and was successfully applied to plasma and brain samples obtained from rats treated with a 10 mg/kg single oral dose of GF449, thus demonstrating its applicability to preclinical pharmacokinetic studies.
Subject(s)
Amines/analysis , Blood Chemical Analysis/methods , Brain , Chromatography, Liquid/methods , Ethylamines/analysis , Heterocyclic Compounds, 1-Ring/analysis , Serotonin 5-HT1 Receptor Agonists/analysis , Tandem Mass Spectrometry/methods , Amines/blood , Animals , Calibration , Ethylamines/blood , Heterocyclic Compounds, 1-Ring/blood , Limit of Detection , Linear Models , Rats , Serotonin 5-HT1 Receptor Agonists/bloodABSTRACT
Sensing technology is the key of intelligent packaging. A variety of different sensing systems for indicating freshness through intelligent packaging have been presented. Polyaniline (PANI) can change its color reversibly through the acid-base reaction with reactive compounds and has been widely used in different kinds of sensors. However, because PANI is insoluble in common organic solvents, this limits its practical usage in many applications. In this work, a highly stable polyaniline-poly(sodium 4-styrenesulfonate) (PANI:PSS) colloid has been developed as a facile colorimetric sensor of volatile amines. The results showed the PANI:PSS colloid is quite sensitive to changes in pH. When PANI:PSS colloids were homogenously deposited on filter paper, the paper are used as a sensor to detect triethylamine (TEA) vapor. The green color of the test paper changed to blue at a TEA concentration as low as 188 ppm.
Subject(s)
Aniline Compounds/chemistry , Ethylamines/analysis , Nanoparticles/chemistry , Polymers/chemistry , Sulfonic Acids/chemistry , Colloids , Colorimetry/methods , Food Analysis , Spectrophotometry, UltravioletABSTRACT
A gas chromatography-electron impact-tandem mass spectrometric method was established for the simultaneous determination of seven adulterants, including fenfluramine (FEN), norpseudoephedrine (NPE), pseudoephedrine (PSE), ephedrine (EPH), amfepramone (AMF), sibutramine (SIB) and strychnine (STR) in slimming functional foods. The target chemicals were extracted with 2% formic acid solution and then cleaned-up with solid-phase extraction using a strong cation exchange cartridge from tablet, liquid, mixed plant powder and capsule formulations. Chromatographic separation was accomplished on a VF-5MS column within 23 min. Leucomalachite green was employed as an internal standard. The recoveries of seven target chemicals in two formulations ranged from 80.1 to 106%. Limits of detection of the method were from 7.5 to 375 µg/kg with relative standard deviations of 1.6 to 13.9%. The linearity of the method ranged from 90 to 1500 ng/mL for NPE, 150 to 1500 ng/mL for STR, 10 to 500 ng/mL for AMF, 5.0 to 500 ng/mL for PSE and EPH and 3.0 to 500 ng/mL for FEN and SIB. This method was applied to the determination of six brands of slimming functional foods. SIB was detected in five of the samples with the contents in the range of 10.3 - 8.55 × 10(5) µg/kg.
Subject(s)
Appetite Depressants/analysis , Drug Contamination , Foods, Specialized/analysis , Gas Chromatography-Mass Spectrometry/methods , Tandem Mass Spectrometry/methods , Capsules/chemistry , Cyclobutanes/analysis , Ethylamines/analysis , Limit of Detection , Linear Models , Reproducibility of Results , Solid Phase Extraction , Strychnine/analysis , Tablets/chemistryABSTRACT
A new multi-channel purge and trap system coupled with ion chromatography for the determination of six alkylamines in cosmetics was developed. The proposed method, based on purge and trap of the volatile alkylamines, involved in a miniaturization and multi-channel integration of classical steam distillation and a simple approach for routine labs. The procedure was rapidly achieved within 10 min and the matrix interferences could be effectively eliminated. Sample pretreatment frequency was higher than 40 h(-1). The linear ranges were 0.1-15 mg L(-1) and the detection limits varied from 0.023 to 0.038 mg L(-1). This method was successfully utilized to determine the amounts of alkylamines in cosmetics with recoveries ranging from 80.3 to 105.5% and the relative standard deviations (RSDs) ranging from 0.78 to 7.5%. It was proved to be accurate, time-saving, and suitable for the determination of large numbers of cosmetics in a short time.
Subject(s)
Amines/analysis , Chromatography, Ion Exchange/instrumentation , Cosmetics/chemistry , Butylamines/analysis , Chromatography, Ion Exchange/methods , Ethylamines/analysis , Humans , Limit of Detection , Methylamines/analysis , Propylamines/analysisABSTRACT
Small molecule microarrays (SMMs) are proving to be increasingly important tools for assessing protein-ligand interactions, as well as in screening for enzyme substrates and inhibitors, in a high-throughput manner. We previously described an SMM-facilitated screening strategy for the rapid identification of probes against γ-secretase, an aspartic protease. In this article, we extend upon this work with an expanded library of hydroxyethylamine-derived inhibitors which non-exclusively target aspartic proteases. Our library is diversified across P(2), P(1), P(1)', and P(2)' positions. Accordingly, 86 new inhibitors are synthesized using a combinatorial, solid-phase synthetic approach, bringing the total library size to 284-biotinylated compounds, which were arrayed onto avidin slides. In order to elucidate enzymatic activity and profiles within complex biological samples, screening is performed using fluorescently-labeled mammalian cell lysates. This yielded reproducible profiles or binding fingerprints that correspond with interactions from aspartic proteases or accessory proteins as well as other interacting targets that were present in the sample. The brightest microarray hits were converted to affinity-based probes (AfBPs) using convenient, 1-step "click" chemistry with benzophenone from the relevant building blocks. Pull-down/mass spectrometric analysis with these probes (individuals or cocktail) yielded putative protein targets that include well-known aspartic proteases, such as cathepsinâ D which is a clear marker for breast cancer cell lines, T47D. Many other hits were also identified, which may be secondary or tertiary interactors of aspartic proteases, or yet unreported off-targets of the hydroxyethylamine pharmacophore. Our work herein thus provides a candidate list of biomarkers for further investigations. Taken together, this SMM-facilitated strategy for the discovery of new AfBPs should provide a useful tool for high-throughput development of novel small molecule probes and the identification of new aspartic proteases as well as related biomarkers in the future.
Subject(s)
Affinity Labels , Cell Extracts/chemistry , Microarray Analysis/methods , Proteome/analysis , Small Molecule Libraries/analysis , Aspartic Acid Proteases/antagonists & inhibitors , Aspartic Acid Proteases/metabolism , Biomarkers/analysis , Cell Line, Tumor , Click Chemistry , Ethylamines/analysis , Ethylamines/chemical synthesis , Ethylamines/chemistry , Ethylamines/pharmacology , Humans , Molecular Probes/analysis , Molecular Structure , Protease Inhibitors/analysis , Protease Inhibitors/chemical synthesis , Protease Inhibitors/chemistry , Protease Inhibitors/pharmacology , Small Molecule Libraries/chemical synthesis , Small Molecule Libraries/chemistry , Small Molecule Libraries/pharmacology , Stereoisomerism , Structure-Activity RelationshipABSTRACT
A simple and rapid reversed phase liquid chromatographic method for separation and determination of the related substances of telmisartan (TLM) was developed and validated. The chromatographic separation was achieved on Lichrospher RP-18 column (250 × 4.6 mm, 5 µm), using 20 mM ammonium acetate containing 0.1% (v/v) triethylamine (pH adjusted to 3.0 with trifluoroacetic acid) and acetonitrile as mobile phase at 25°C. The detection was performed at 254 nm. The method was validated and found to be robust, precise, specific and linear between 0.37 and 500 µg/mL. The limits of detection and quantification of telmisartan were 0.11 and 0.37 µg/mL, respectively. The method was successfully applied to quantify related substances and assay of TLM in bulk drugs and commercial tablets. The related substances relate to a novel synthetic route and different from those A-H impurities reported by European Pharmacopeia.