Gene/Protein Disease Symptom Drug Enzyme Compound
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A simple and rapid procedure for the separation and determination of inorganic, methyl, and ethyl mercury compounds was described using liquid chromatography (LC) followed by vapor generation inductively coupled plasma-mass spectrometry (VG-ICP-MS). Well resolved chromatograms were obtained within 5 min by reversed-phase liquid chromatography with a C8 column as the stationary phase and a pH 4.7 solution containing 0.5% v/v 2-mercaptoethanol and 5% v/v methanol as the mobile phase. The separated mercury compounds were converted to mercury vapors by an in situ nebulizer/vapor generation system for their introduction into ICP. The concentrations of NaBH4 and HNO3 required for vapor generation were also optimized. The method was applied for the speciation of mercury in reference materials NIST SRM 1568a Rice Flour and NIST SRM 1567a Wheat Flour and also rice flour and wheat flour samples purchased locally. The accuracy of the procedure was verified by analyzing the certified reference material NRCC DOLT-3 Dogfish Liver for methyl mercury. Precision between sample replicates was better than 13% for all the determinations. The detection limits of the mercury compounds studied were in the range 0.003-0.006 ng Hg mL(-1) in the injected solutions, which correspond to 0.02-0.06 ng g(-1) in original flour samples. A microwave-assisted extraction procedure was adopted for the extraction of mercury compounds from rice flour, wheat flour, and fish samples using a mobile phase solution.
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PMID:Speciation analysis of mercury in cereals by liquid chromatography chemical vapor generation inductively coupled plasma-mass spectrometry. 1864 58

Cadmium, lead and copper were determined in synthetic sea-water, drinking water and the NBS 1643b Trace Elements in Water standard reference material at mug/l. levels by flame atomic-absorption spectrometry after on-line preconcentration by sorbent extraction with a flow-injection system. Bonded silica with octadecyl functional groups packed in a micro column of 100 mul capacity was used to collect diethylammonium diethyldithiocarbamate complexes of the heavy metals in the aqueous samples. The sample loading time was 20 sec at a flow-rate of 3.3 ml/min. Ethanol or methanol was used to elute the adsorbed analytes into the spectrometer. The sample loading rate, elution rate and pH were optimized. Enrichment factors of 19-25 for Cd, Pb and Cu were achieved at sampling frequencies of 120/hr with precisions of 1.4, 1.0 and 1.3% rsd (n = 11), respectively. The detection limits (3sigma) for Cd, Pb and Cu were 0.3, 3 and 0.2 mug/l., respectively. Determination of Cd, Pb and Cu in NBS SRM 1643b showed good agreement with the certified values. Recoveries of Cd and Pb added to sea-water were 95 and 102%, respectively.
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PMID:Determination of cadmium, lead and copper in water samples by flame atomic-absorption spectrometry with preconcentration by flow-injection on-line sorbent extraction. 1896 93

Inorganic arsenic species are metabolized to monomethylarsonic acid (MMA(V)) and dimethylarsinic acid (DMA(V)) and excreted into urine. A simple, rapid and sensitive method has been developed using electrospray ionization tandem mass spectrometry (ESI-MS-MS) for the simultaneous determination of MMA(V) and DMA(V). MMA(V) and DMA(V) in a sample were allowed to react with citric acid (CiA). Adduct compounds were extracted together with isoamyl alcohol (IAA). An aliquot (1-microL) of the IAA layer was directly injected into the ESI-MS-MS instrument, and was detected within 1 min. Quantification was done using selected reaction monitoring for MMA(V) and DMA(V) as follows: [MMAH + 2CiA - 3H(2)O](+) --> [MMAH + CiA - 2H(2)O](+) [DMAH + CiA + MeOH - 2H(2)O](+) --> [DMAH + MeOH - H(2)O](+) where MMAH and DMAH denote the protonated forms of MMA(V) and DMA(V), and MeOH denotes methanol (carrier liquid in ESI-MS-MS). This method was validated for the analysis of urine samples. The limit of detection of As was 0.3 microg L(-1) for MMA(V) and 0.6 microg L(-1) for DMA(V) using 10 microL of sample solution. Results were obtained in <10 min with a linear calibration range of 3-100 microg L(-1). Inorganic arsenic compounds (and other organic arsenic compounds) found in urine did not interfere with the detection of MMA(V) and DMA(V). Concentrations of MMA(V) and DMA(V) in the reference urine SRM 2670a were estimated after partial purification, and those in urine of a patient treated with As(2)O(3) were measured after dilution.
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PMID:Electrospray ionization tandem mass spectrometric determination of monomethylarsonic acid and dimethylarsinic acid after adduct formation with citric acid. 1932 67

Soot has been considered as a potentially important sorbent for organic contaminants in soils, sediments, and aerosols. This paper demonstrates that native (authigenic) extractable organic material (EOM) and surface-covering water on soot may have a substantial influence on sorption properties of the soot. Sorption isotherms were determined for apolar and weakly polar sorbates (n-octane, cyclooctane, n-propylbenzene, naphthalene) from an aqueous solution to a standard reference material of diesel soot (SRM 2975) in the original state and after extraction with methanol. For all sorbates tested, removal of EOM from soot by methanol caused the sorption isotherms to be more nonlinear (decrease of Freundlich exponents by 0.19-0.25) compared to the untreated soot. The changes in the isotherms depend on both sorbate structure and sorbate concentration and can be accounted for by two opposing roles that EOM could have on the sorption properties of soot (i) enhancing the overall sorption by absorbing the sorbate into the EOM phase, and (ii) attenuating the sorbate adsorption to the soot carbon surface through sorption competition or site blockage. The n-alkane-to-cycloalkane sorption coefficient ratios (Kn/Kc) indicated that the removal of EOM altered the sorption mode for alkanes from absorption to adsorption. A comparison of the sorption isotherms measured in aqueous suspensions with the soot-air sorption coefficients reported for SRM 2975 in the literature showed that sorption to "soot in water" is significantly weaker than sorption to "soot in air", indicating that complete surface coverage with water suppresses the sorption by soot.
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PMID:Effects of native organic material and water on sorption properties of reference diesel soot. 1967 23

A procedure was developed for the quantitative determination of chafuroside A, a flavone C-glycoside with potent anti-inflammatory activity, and its regioisomer chafuroside B, as well as isovitexin and vitexin, by selected reaction monitoring liquid chromatography-tandem mass spectrometry (SRM LC-MS/MS) analysis. This method was successfully applied to commercial leaves of green tea, houji tea, oolong tea, and black tea. High levels of chafurosides A and B were found in oolong tea leaves that had been heated at >140 degrees C. Next, their precursors, prechafurosides A and B, were isolated from methanol extract of oolong tea leaves prepared from Shizu 7132, Camellia sinensis (L.) O. Kuntze, by partition with n-butanol and H2O and chromatography on Diaion SP-825, Sephadex LH-20, and ODS C-18, guided by assay of chafuroside formation. Prechafurosides A and B gave chafurosides A and B, respectively, in good yields when heated at 160 degrees C for 0.5 h. Solvolysis of prechafurosides A and B with pyridine and dioxane quantitatively afforded isovitexin and vitexin, respectively. On the basis of these results and physicochemical data (MS, UV, and NMR), prechafurosides A and B were concluded to be new flavone C-glycoside sulfates, isovitexin-2''-sulfate and vitexin-2''-sulfate, respectively.
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PMID:Quantitation of chafurosides A and B in tea leaves and isolation of prechafurosides A and B from oolong tea leaves. 1957 51

A total of 14 tetra- to deca- PBDE congeners were separated on a C(18) reversed phase liquid chromatographic column. PBDEs 47, 85, 99, 100, 153, 154, 183, 196, 197, 203, 206, 207, 208, and 209 were eluted using a gradient methanol/water/toluene mobile phase system at a flow rate of 0.5 mL min(-1). (13)C-BDE-47, (13)C-BDE-99, (13)C-BDE-153, BDE-128, and (13)C-BDE-209 were used as internal standards, while (13)C-BDE-100 was used as a syringe standard. Separated analytes were ionized using an atmospheric pressure photoionization (APPI) source equipped with a 10 eV krypton lamp and operated in negative ion mode. [M-Br + O](-) ions were monitored as precursor ions for all studied PBDEs, except for BDE-208 and BDE-209 which produced higher intensity at the [C(6)Br(5)O](-) ion cluster. [Br](-) ions were monitored as fragment ions for all target compounds. Method detection limits ranged from 12 to 30 pg. The method was applied to determination of PBDEs in standard reference material (SRM 2585), and favorable results were obtained. Unlike GC methods, no thermal degradation was encountered in the analysis of higher brominated PBDEs. This rendered the method useful for quantification of BDE-209 debromination products. The method also allows the use of (13)C-labeled internal standards, which compensate for instrumental fluctuations and matrix-related ion suppression or enhancement.
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PMID:Isotope dilution method for determination of polybrominated diphenyl ethers using liquid chromatography coupled to negative ionization atmospheric pressure photoionization tandem mass spectrometry: validation and application to house dust. 1971 67

An automated hydride generation (AHG) interface to inductive coupled plasma mass spectroscopy (ICPMS) was developed for measuring arsenic in environmental samples. This technique provides statistically indistinguishable response slopes (within about 3%) for hydride generation-ICPMS (HG-ICPMS) analysis of all major As species, inorganic As(III), dimethylarsinic acid (DMA), monomethylarsonic acid (MMA), and inorganic As(V); this has not previously been achieved. Previously, sample pretreatment to convert all forms of As into As(V) has been a prerequisite for measuring total arsenic in complex matrices. Under our operating conditions, arsenobetaine (AsB), until now regarded to be inert, also generates a hydride (albeit the response is only approximately 7% of others). The limit of detection (LOD) based on three times the standard deviation of the blank with this technique for AsB, DMA, As(III), MMA, and As(V) is 90, 66, 63, 63, and 63 pg As, respectively. This AHG-ICPMS technique was compared with a flow injection-UV photolysis-HG-ICPMS (FI-UV-ICPMS) and liquid chromatography-UV-HG-ICPMS analysis of arsenic content in National Institute of Standards & Technology (NIST) standard rice flour (standard reference material: SRM 1568a) and rice samples collected from West Bengal, India. Both oxidative acid digestion and methanol:water (1:1) extraction were used. The analytical results for total As in the SRM 1568a digest were 99.2 +/- 0.6 and 100.2 +/- 0.8% of the certified value (290 +/- 3 microg As/kg) by the AHG-ICPMS and the FI-UV-HG-ICPMS techniques, respectively. For rice extracts and the digests, the two techniques provided results that were correlated with linear r2 values of 0.9988 and 0.9987 with intercepts statistically indistinguishable from zero. Chromatographic analysis indicated that As in these rice samples were 75-90% inorganic.
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PMID:An automated hydride generation interface to ICPMS for measuring total arsenic in environmental samples. 1989 55

7-Carboxymethylguanine (7-CMGua) and 7-(2'-carboxyethyl)guanine (7-CEGua) are DNA adducts that potentially could be formed upon the metabolism of the carcinogenic nitrosamines N-nitrososarcosine (NSAR) and 3-(methylnitrosamino)propionic acid (MNPA), respectively, or from other sources such as nitrosation of glycine (7-CMGua) or reaction of DNA with acrylic acid (7-CEGua). Since both NSAR and MNPA have been detected in human urine and there are plausible sources of exposure to other precursors to these adducts, we analyzed human liver DNA for 7-CMGua and 7-CEGua, using liquid chromatography-electrospray ionization-tandem mass spectrometry-selected reaction monitoring (LC-ESI-MS/MS-SRM). Human hepatic DNA was mixed with [15N5]7-CMGua and [15N5]7-CEGua as internal standards and enzymatically hydrolyzed. The hydrolysate was partially purified by solid-phase extraction, and the resulting fraction was treated with acetyl chloride in methanol to convert 7-CMGua and 7-CEGua to their methyl esters. After a second solid-phase extraction, LC-ESI-MS/MS-SRM analysis was carried out using the transitions m/z 224 [M + H](+) --> m/z 164 [(M + H)-HCOOCH3]+ and m/z 238 [M + H]+ --> m/z 152 [BH]+ for the methyl esters of 7-CMGua and 7-CEGua, respectively. The method was sensitive, accurate, precise, and apparently free from artifact formation. 7-CEGua, as its methyl ester, was detected in all 24 human liver samples analyzed, mean +/- SD, 373 +/- 320 fmol/mumol Gua (74.6 adducts per 10(9) nucleotides), range 17-1189 fmol/mumol Gua, but the methyl ester of 7-CMGua was not detected in any sample. These results demonstrate the ubiquitous presence of 7-CEGua in human liver DNA. Acrylic acid may be a likely endogenous precursor to 7-CEGua.
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PMID:Detection of 7-(2'-carboxyethyl)guanine but not 7-carboxymethylguanine in human liver DNA. 2043 65

UHPLC-MS/MS method using BEH C18 analytical column was developed for the separation and quantitation of 12 phenolic compounds of Chamomile (Matricaria recutita L.). The separation was accomplished using gradient elution with mobile phase consisting of methanol and formic acid 0.1%. ESI in both positive and negative ion mode was optimized with the aim to reach high sensitivity and selectivity for quantitation using SRM experiment. ESI in negative ion mode was found to be more convenient for quantitative analysis of all phenolics except of chlorogenic acid and kaempherol, which demonstrated better results of linearity, accuracy and precision in ESI positive ion mode. The results of method validation confirmed, that developed UHPLC-MS/MS method was convenient and reliable for the determination of phenolic compounds in Chamomile extracts with linearity >0.9982, accuracy within 76.7-126.7% and precision within 2.2-12.7% at three spiked concentration levels. Method sensitivity expressed as LOQ was typically 5-20 nmol/l. Extracts of Chamomile flowers and Chamomile tea were subjected to UHPLC-MS/MS analysis. The most abundant phenolic compounds in both Chamomile flowers and Chamomile tea extracts were chlorogenic acid, umbelliferone, apigenin and apigenin-7-glucoside. In Chamomile tea extracts there was greater abundance of flavonoid glycosides such as rutin or quercitrin, while the aglycone apigenin and its glycoside were present in lower amount.
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PMID:Development and application of UHPLC-MS/MS method for the determination of phenolic compounds in Chamomile flowers and Chamomile tea extracts. 2080 28

A simple, cost effective, and yet sensitive sample preparation technique was investigated for determining Polycyclic Aromatic Hydrocarbons (PAHs) in solid samples. The method comprises ultrasonic extraction, Stir Bar Sorptive Extraction (SBSE), and thermal desorption-gas chromatography-mass spectrometry to increase analytical capacity in laboratories. This method required no clean-up, satisfied PAHs recovery, and significantly advances cost performance over conventional extraction methods, such as Soxhlet and Microwave Assisted Extraction (MAE). This study evaluated three operational parameters for ultrasonic extraction: solvent composition, extraction time, and sample load. A standard material, SRM 1649 a (urban dust), was used as the solid sample matrix, and 12 priority PAHs on the US Environmental Protection Agency (US EPA) list were analyzed. Combination of non-polar and polar solvents ameliorated extraction efficiency. Acetone/hexane mixtures of 2:3 and 1:1 (v/v) gave the most satisfactory results: recoveries ranged from 63.3% to 122%. Single composition solvents (methanol, hexane, and dichloromethane) showed fewer recoveries. Comparing 20 min with 60 min sonication, longer sonication diminished extraction efficiencies in general. Furthermore, sample load became a critical factor in certain solvent systems, particularly MeOH. MAE was also compared to the ultrasonic extraction, and results determined that the 20-min ultrasonic extraction using acetone/hexane (2:3, v/v) was as potent as MAE. The SBSE method using 20 mL of 30% alcohol-fortified solution rendered a limit of detection ranging from 1.7 to 32 ng L(-1) and a limit of quantitation ranging from 5.8 to 110 ng L(-1) for the 16 US EPA PAHs.
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PMID:A cost effective, sensitive, and environmentally friendly sample preparation method for determination of polycyclic aromatic hydrocarbons in solid samples. 2085 99


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