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Results for “Journal of Chromatography A”

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USGS2020

Combined extraction-cleanup column chromatographic procedure for determination of dicofol in avian eggs

Dicofol in avian eggs was completely oxidized to dichlorobenzophenone (DCBP) when a hexane Soxhlet extraction procedure was used. This degradation did not occur with other avian tissues (muscle and liver). For this reason, a combined extraction-cleanup column chromatographic procedure, without added heat, was developed for the determination of dicofol in avian eggs. Homogenized subsamples of eggs were mixed with sodium sulfate, and the mixture was added as the top layer on a column prepacked with Florisil. The dicofol and other compounds of interest were then eluted with ethyl etherhexane. The extracts, relatively free from lipids, were quantitated on a gas chromatograph equipped with a 63Ni electron-capture detector and a methyl silicone capillary column. Recoveries from chicken eggs, fortified with dicofol and other DDT-related compounds, averaged 96%. Analysis of eggs of eastern screech-owls, fed a meat diet containing 10 ppm technical Kelthane, showed that both dicofol and DCBP were present. Results were confirmed by gas chromatography/ mass spectrometry. This method is rapid and reliable, involves a minimum of sample handling, and is well suited for high volume determination of dicofol in eggs and other avian tissues .

Journal of the Association of Official Analytical ↗

USGS2006

A laboratory and field evaluation of a portable immunoassay test for triazine herbicides in environmental water samples

The usefulness and sensitivity, of a portable immunoassay test for the semiquantitative field screening of water samples was evaluated by means of laboratory and field studies. Laboratory results indicated that the tests were useful for the determination of atrazine concentrations of 0.1 to 1.5 μg/L. At a concentration of 1 μg/L, the relative standard deviation in the difference between the regression line and the actual result was about 40 percent. The immunoassay was less sensitive and produced similar errors for other triazine herbicides. After standardization, the test results were relatively insensitive to ionic content and variations in pH (range, 4 to 10), mildly sensitive to temperature changes, and quite sensitive to the timing of the final incubation step, variances in timing can be a significant source of error. Almost all of the immunoassays predicted a higher atrazine concentration in water samples when compared to results of gas chromatography. If these tests are used as a semiquantitative screening tool, this tendency for overprediction does not diminish the tests' usefulness. Generally, the tests seem to be a valuable method for screening water samples for triazine herbicides.

International Journal of Environmental Analytical ↗

USGS2020

Semiquantitative determination of polychlorinated biphenyls in tissue samples by thin layer chromatography

A method is described for the analysis of polychlorinated biphenyl (PCB) compounds in tissue samples. Cleanup by hexane-acetonitrile partitioning and Florisil column chromatography are performed on samples before oxidative treatment to convert DDE to DCBP. PCB components are then determined semi-quantitatively by TLC. No prior separation of PCB from chlorinated pesticides is required. The lower limit of sensitivity is 0.2 μ g.

Journal of the Association of Official Analytical ↗

USGS1986

Persistence of rotenone in ponds at different temperatures

Two ponds were treated with liquid rotenone (5% rotenone), one with 3 mg/L at 24°C and the other with 2 mg/L at 0°C (concentrations of active rotenone were 0.15 and 0.10 mg/L, respectively). Water samples were collected and analyzed by high-performance liquid chromatography. The concentration of rotenone declined to 0.02 mg/L in 48 h in warm water and in 11 d in cold water. The half-life of rotenone was calculated at 13.9 h in warm water and 83.9 h in cold water.

North American Journal of Fisheries Management↗

USGS1973

A study of the distribution of the polychlorinated biphenyls in the aquatic environment

Data gathered from monitoring activities and project studies indicate the ubiquitous occurrence and distribution of polychlorinated biphenyls in the aquatic environment. Residues have been detected in samples from 19 States, representing nearly every region of the country. Concentrations ranged from 0.1 to 4.0 ug/l in unfiltered water samples and 5.0 to 3,200 ug/kg in bottom sediments. PCB residues were also found in fish and aquatic plants. Samples were prepared by the same techniques used for general chlorinated insecticide detection, with special attention to cleanup and separation of PCB's from other compounds. Basic identification and quantification were made by dual-column electron-capture gas chromatography and confirmed by gas chromatography mass spectrometry whenever possible. The sampling program is expected to be broadened geographically in 1973 and increased in successive years in order to more adequately define the distribution of PCB residues in the major drainage basins of the United States.

Journal of Research of the U.S. Geological Survey↗

USGS1989

Characterization of coal-derived hydrocarbons and source-rock potential of coal beds, San Juan Basin, New Mexico and Colorado, U.S.A.

Coal beds are considered to be a major source of nonassociated gas in the Rocky Mountain basins of the United States. In the San Juan basin of northwestern New Mexico and southwestern Colorado, significant quantities of natural gas are being produced from coal beds of the Upper Cretaceous Fruitland Formation and from adjacent sandstone reservoirs. Analysis of gas samples from the various gas-producing intervals provided a means of determining their origin and of evaluating coal beds as source rocks. The rank of coal beds in the Fruitland Formation in the central part of the San Juan basin, where major gas production occurs, increases to the northeast and ranges from high-volatile B bituminous coal to medium-volatile bituminous coal ( R m values range from 0.70 to 1.45%). On the basis of chemical, isotopic and coal-rank data, the gases are interpreted to be thermogenic. Gases from the coal beds show little isotopic variation ( δ 13 C 1 values range −43.6 to −40.5 ppt), are chemically dry (C 1 /C 1–5 values are > 0.99), and contain significant amounts of CO 2 (as much as 6%). These gases are interpreted to have resulted from devolatilization of the humic-type bituminous coal that is composed mainly of vitrinite. The primary products of this process are CH 4 , CO 2 and H 2 O. The coal-generated, methane-rich gas is usually contained in the coal beds of the Fruitland Formation, and has not been expelled and has not migrated into the adjacent sandstone reservoirs. In addition, the coal-bed reservoirs produce a distinctive bicarbonate-type connate water and have higher reservoir pressures than adjacent sandstones. The combination of these factors indicates that coal beds are a closed reservoir system created by the gases, waters, and associated pressures in the micropore coal structure. In contrast, gases produced from overlying sandstones in the Fruitland Formation and underlying Pictured Cliffs Sandstone have a wider range of isotopic values ( δ 13 C 1 values range from −43.5 to −38.5 ppt), are chemically wetter (C 1 /C 1–5 values range from 0.85 to 0.95), and contain less CO 2 (< 2%). These gases are interpreted to have been derived from type III kerogen dispersed in marine shales of the underlying Lewis Shale and nonmarine shales of the Fruitland Formation. In the underlying Upper Cretaceous Dakota Sandstone and Tocito Sandstone Lentil of the Mancos Shale, another gas type is produced. This gas is associated with oil at intermediate stages of thermal maturity and is isotopically lighter and chemically wetter at the intermediate stage of thermal maturity as compared with gases derived from dispersed type III kerogen and coal; this gas type is interpreted to have been generated from type II kerogen. Organic matter contained in coal beds and carbonaceous shales of the Fruitland Formation has hydrogen indexes from Rock-Eval pyrolysis between 100 and 350, and atomic H:C ratios between 0.8 and 1.2. Oxygen indexes and atomic O:C values are less than 24 and 0.3, respectively. Extractable hydrocarbon yields are as high as 7,000 ppm. These values indicate that the coal beds and carbonaceous shales have good potential for the generation of liquid hydrocarbons. Voids in the coal filled with a fluorescent material that is probably bitumen is evidence that liquid hydrocarbon generation has taken place. Preliminary oil-source rock correlations based on gas chromatography and stable carbon isotope ratios of C 15+ hydrocarbons indicate that the coals and (or) carbonaceous shales in the Fruitland Formation may be the source of minor amounts of condensate produced from the coal beds at relatively low levelsof thermal maturity ( R m =0.7).

International Journal of Coal Geology↗

USGS1982

Organophosphate insecticide poisoning of Canada geese in the Texas panhandle

Sixteen hundred waterfowl, mostly Canada Geese, died near Etter, Texas, in late January 1981 from anticholinesterase poisoning. Winter wheat in the area of the die-off had been treated with organophosphate insecticides to control greenbugs. Cholinesterase (ChE) levels in brains of a sample of geese found dead were 75% below normal, enough to account for death (Ludke et al. 1975). The gastrointestinal (G I) tracts of geese found dead were packed with winter wheat; gas chromatography techniques identified parathion and methyl parathion in the GI tract contents. Residues of both chemicals were confirmed by mass spectrometry. We recommend that less toxic materials, such as malathion, be used on grain crops when waterfowl are in the vicinity of treatment.

Texas↗

USGS2020

Gas-liquid chromatographic determination of kepone in field-collected avian tissues and eggs

A procedure is described for determining Kepone (decachlorooctahydro-l,3,4-metheno-2H-cyclobuta [cd]pentalene-2-one) residues in avian egg, liver, and tissue. Samples were extracted with benzene-isopropanol, and the extract was cleaned up with fuming H 2 SO 4 -concentrated H 2 SO 4 . Kepone was separated from organochlorine pesticides and polychlorinated biphenyls on a Florisil column and analyzed by electron capture gas-liquid chromatography GLC). The average recovery from spiked tissues was 86%. The analyses performed on 14 bald eagle carcasses and livers, 3 bald eagle eggs, and 14 osprey eggs show measurable levels which indicate that Kepone accumulates in the tissues of fish-eating birds. Residues were confirmed by GLC-mass spectrometry.

Journal of the Association of Official Analytical ↗

USGS2020

Liquid-chromatographic determination of sarafloxacin residues in channel catfish muscle-tissue

A liquid chromatographic method is described for the determination of sarafloxacin hydrochloride residues in channel catfish ( Ictalurus punctatus ) fillets. Sarafloxacin was extracted from fillet tissue with acetonitrile–water (1+1). The extract was centrifuged and the supernatant was partitioned with hexane. The aqueous fraction was filtered through a 0.45 μm filter and evaporated to dryness. The sample was redissolved with 20% acetonitrile–methanol (3 + 2) and 80% trifluoroacetic acid (0.1%), centrifuged, and filtered to remove proteins. Samples were analyzed by chromatography with gradient elution on a C 18 column and with fluorescence detection (excitation at 280 nm and emission above 389 nm). Mean recoveries ranged from 85.4 to 104%, and relative standard deviations ranged from 1.06 to 5.58% in samples spiked at concentrations of 10.0–863.8 ng/g. The method detection limit for sarafloxacin was 1.4 ng/g.

Journal of AOAC International↗

USGS1995

Application of brain cholinesterase reactivation to differentiate between organophosphorus and carbamate pesticide exposure in wild birds

Brain cholinesterase activity was measured to evaluate pesticide exposure in wild birds. Thermal reactivation of brain cholinesterase was used to differentiate between carbamate and organophosphorus pesticide exposure. Brain cholinesterase activity was compared with gas chromatography and mass spectrometry of stomach contents. Pesticides were identified and confirmed in 86 of 102 incidents of mortality from 29 states within the USA from 1986 through 1991. Thermal reactivation of cholinesterase activity was used to correctly predict carbamates in 22 incidents and organophosphates in 59 incidents. Agreement ( P < 0.001) between predictions based on cholinesterase activities and GC/MS results was significant.

Journal of Wildlife Diseases↗

USGS2020

Liquid-chromatographic determination of rotenone in fish, crayfish, mussels, and sediments

An analytical procedure is described for determining residues of rotenone in fish muscle, fish offal, crayfish, freshwater mussels, and bottom sediments. Tissue samples were extracted with ethyl ether and extracts were cleaned up by gel permeation chromatography and silica gel chromatography. Sediment samples were extracted with methanol, acidified, partitioned into hexane, and cleaned up on a silica gel column. Rotenone residues were quantitated by liquid chromatography, using ultraviolet (295 nm) detection. Recoveries from sediment samples fortified with rotenone at 0.3 μg/g were 80.8%, whereas recoveries from tissue samples fortified with 0.1 μg/g ranged from 87.7 to 96.8%. Samples fortified with 0.3 μg/g and stored at - 10°C for 6 months before analysis had recoveries ranging from 83.2 to 90.5%. Limits of detection were 0.025 μg/g for sediments and 0.005 μg/g for tissue samples.

Journal of the Association of Official Analytical ↗

USGS1967

Insecticide residues in big game mammals of South Dakota

An analysis was made of eight insecticide residues in the renal fat tissue of 23 white-tailed deer ( Odocoileus virginianus ), 13 mule deer ( O. hemionus ), 9 pronghorns ( Antilocapra americana ), and 2 elk ( Cervus canadensis ) collected in South Dakota during the fall of 1964. Identification and quantitative analysis of the insecticide residues were accomplished by thin-layer and gas-liquid chromatography. Eighty-five percent of the samples had residues of DDT with an average of 0.13 ppm. DDD residues were found in 11 percent of the samples, DDE in 38 percent, dieldrin in 38 percent, and lindane in 15 percent, with an average of 0.07, 0.04, 0.03, and 0.04 ppm, respectively. Heptachlor, heptachlor epoxide, and aldrin were not detected in concentrations above the limits of the experiment set by the investigators.

South Dakota↗

USGS2005

Acute toxicity of resmethrin, malathion and methoprene to larval and juvenile American lobsters ( Homarus amemcanus ) and analysis of pesticide levels in surface waters after Scourge™, Anvil™ and Altsoid™ application

Acute toxicity and immune response, combined with temperature stress effects, were evaluated in larval and juvenile American lobsters ( Homarus americanus ) exposed to malathion, resmethrin and methoprene. These pesticides were used to control West Nile virus in New York in 1999, the same year the American lobster population collapsed in western Long Island Sound (LIS). Whereas the suite of pesticides used for mosquito control changed in subsequent years, a field study was also conducted to determine pesticide concentrations in surface waters on Long Island and in LIS after operational applications. The commercial formulations used in 2002 and 2003—Scourge, Anvil and Altosid—contain the active ingredients resmethrin, sumithrin and methoprene, respectively. Concentrations of the synergist piperonyl butoxide (PBO) were also measured as a proxy for pesticide exposure. Acute mortality in Stage I-II larval lobsters demonstrated that they are extremely sensitive to continuous resmethrin exposure. Resmethrin LC50s for larval lobsters determined under flow-through conditions varied from 0.26–0.95 μg L −1 in 48- and 96-h experiments at 16°C, respectively. Increased temperature (24°C) did not significantly alter resmethrin toxicity. Malathion and methoprene were less toxic than resmethrin. The 48-h LC50 for malathion was 3.7 μg L −1 and methoprene showed no toxicity at the highest (10 μg L −1 ) concentration tested. Phenoloxidase activity was used as a measure of immune response for juvenile lobsters exposed to sublethal pesticide concentrations. In continuous exposures to sublethal doses of resmethrin (0.03 μg L −1 ) or malathion (1 μg L −1 ) for 7 d at 16 or 22°C, temperature had a significant effect on phenoloxidase activity ( P ≤ 0.006) whereas pesticide exposure did not ( P = 0.880). The analytical methods developed using high performance liquid chromatography coupled to time-of-flight mass spectroscopy (LC-TOF-MS) provided high sensitivity with mass detection limits of 0.1–0.3 ng L −1 . Pesticide levels were often detected in the ng L −1 range in Long Island surface waters and western LIS (except in open waters), but rarely at concentrations found to be toxic in flow-through laboratory exposures, even immediately after spray events.

Journal of Shellfish Research↗

USGS2020

Liquid chromatographic determination of para-toluenesulfonamide in edible fillet tissues from three species of fish

Chloramine-T ( N -sodium- N -chloro- p -toluene-sulfonamide) is a candidate therapeutic drug for treating bacterial gill disease, a predominant disease of a variety of fish species. Research has been initiated to obtain the U.S. Food and Drug Administration’s (FDA) approval for the use of chloramine-T on a variety of fish species. An attribute of a therapeutic aquaculture drug that must be characterized before the FDA approves its use is depletion of the drug’s marker residue (the drug’s parent compound or metabolite of highest concentration in an edible tissue). para -Toluenesulfonamide (p-TSA) is the primary degradation product and marker residue for chloramine-T in rainbow trout. To conduct residue depletion studies for chloramine-T in fish, a robust analytical method sensitive and specific for p-TSA residues in edible fillet tissue from a variety of fish was required. Homogenized fillet tissues from rainbow trout ( Oncorhynchus mykiss ), walleye ( Stizostedion vitreum ), and channel cattish ( Ictalurus punctatus ) were fortified at nominal p-TSA concentrations of 17, 67, 200, 333, and 1000 ng/g. Samples were analyzed by isocratic reversed-phase liquid chromatography (LC) with absorbance detection at 226 nm. Mean recoveries of p-TSA ranged from 77 to 93.17%; relative standard deviations ranged from 1.5 to 14%; method quantitation limits ranged from 13 to 18 ng/g; and method detection limits ranged from 3.8 to 5.2 ng/g. The LC parameters produced p-TSA peaks without coelution of endogenous compounds and excluded chromatographic interference from at least 20 chemicals and drugs of potential use in aquaculture.

Journal of AOAC International↗

USGS2019

Determination of 3-trifluoromethyl-4-nitrophenol and 3-trifluoromethyl-4-nitrophenol glucuronide in edible fillet tissue of rainbow trout and channel catfish by solid-phase extraction and liquid chromatography

3-Trifluoromethyl-4-nitrophenol (TFM) is a pesticide used for the selective control of sea lampreys ( Petromyzon marinus ) in stream and river tributaries of the Great Lakes. To determine concentrations of TFM and TFM glucuronide in the edible fillet tissue of fish during sea lamprey control treatments, an analytical method was developed to determine the concentrations of these residues in rainbow trout ( Oncorhynchus mykiss ; RBT) and channel catfish ( Ictalurus punctatis ; CCF). Homogenized fillets were extracted with methanol–water (80 + 20). TFM and TFM glucuronide were isolated from coextractives by C 18 solid-phase extraction. TFM glucuronide was hydrolyzed to TFM by the addition of β-glucuronidase to the TFM glucuronide extract. The extracts were analyzed separately by liquid chromatography with UV–visible detection. Recoveries from TFM-fortified CCF and RBT tissues were 84.1 and 96.1%, respectively. The method detection limits (MDLs) are 2.4 ng/g for TFM-fortified tissues of CCF and 3 ng/g for those of RBT. Recoveries were 78.8 and 77%from TFM glucuronide-fortified CCF and RBT tissues, respectively. The MDLs for TFM glucuronide-fortified tissues are 3.5 and 6.9 ng/g for CCF and RBT, respectively.

Journal of AOAC International↗

USGS2020

Determination of submicrogram-per-liter concentrations of caffeine in surface water and groundwater samples by solid-phase extraction and liquid chromatography

A method for determining submicrogram-per-liter concentrations of caffeine in surface water and groundwater samples has been developed. Caffeine is extracted from a 1 L water sample with a 0.5 g graphitized carbon-based solid-phase cartridge, eluted with methylene chloride-methanol (80 + 20, v/v), and analyzed by liquid chromatography with photodiode-array detection. The single-operator method detection limit for organic-free water samples was 0.02 μg/L. Mean recoveries and relative standard deviations were 93 ± 13% for organic- free water samples fortified at 0.04 μg/L and 84 ± 4% for laboratory reagent spikes fortified at 0.5 μg/L. Environmental concentrations of caffeine ranged from 0.003 to 1.44 μg/L in surface water samples and from 0.01 to 0.08 μg/L in groundwater samples.

Journal of AOAC International↗

USGS1973

The fractionation of humic acids from natural water systems

Humic acids, the most abundant organic components of natural water systems, are complex mixtures of molecular aggregates of different chemical and physical properties. The first step in the study of such a mixture is the fractionation of the mixture. The most common approach with humic acids is to attempt to obtain a molecular weight fractionation by gel-permeation chromatography. However, since the preponderance of evidence indicates that the components of humic acid do not fulfill the basic criteria of uniform shape and chemical structure necessary for obtaining a molecular fractionation on gel-permeation media, molecular weight distributions in humic acids cannot be evaluated by this method. A fractionation dependent upon chemical structure can be obtained by the manipulation of elution conditions on a gel-permeation column. This procedure provides a beginning in the isolation and identification of discrete components of humic acids.

Journal of Research of the U.S. Geological Survey↗

USGS2002

Rapid loss of lampricide from catfish and rainbow trout following routine treatment

Rainbow trout (Oncorhynchus mykiss) and channel catfish (Ictalurus punctatus) were exposed to 3-trifluoromethyl-4-nitrophenol (TFM) and Bayluscide (niclosamide) during a sea lamprey control treatment of the Ford River, located in the upper peninsula of Michigan. Caged fish were exposed to a nominal concentration of 0.02 mg/L of niclosamide for a period of approximately 12 h. Samples of fillet tissue were collected from each fish species before treatment and at 6, 12, 18, 24, 48, 96, and 192 h following the arrival of the block of chemical at the exposure site. The fish were dissected, homogenized, extracted, and analyzed by high-performance liquid chromatography. The major residues found in the fillet tissues were TFM and niclosamide. Niclosamide concentrations were highest 12 h after arrival of the chemical block for rainbow trout (0.0395 ?? 0.0251 ??g/g) and 18 h after arrival of the chemical block for channel catfish (0.0465 ?? 0.0212 ??g/g). Residues decreased rapidly after the block of lampricide had passed and were below the detection limits in fillets of rainbow trout within 24 h and channel catfish within 96 h after the arrival of the lampricide.

Journal of Agricultural and Food Chemistry↗