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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↗

USGS2008

Analysis of chlorothalonil and three degradates in sediment and soil

A method has been developed for the simultaneous extraction of chlorothalonil and three of its degradates (4-hydroxy-2,5,6-trichloroisophthalonitrile, 1-carbamoyl-3-cyano-4-hydroxy-2,5,6-trichlorobenzene, and 1,3-dicarbamoyl-2,4,5,6-tetrachlorobenzene) from soils and sediments; the compounds were extracted using sonication with acetone and isolation of the parent compound and matrix interferences from the degradates by solid phase extraction (SPE). The chlorothalonil fraction underwent further coextracted matrix interference removal with Florisil. The degradates were derivatized with N , O- bis(trimethylsilyl) trifluoroacetamide (BSTFA) and chlorotrimethylsilane (TMCS). All compounds were analyzed by gas chromatography–mass spectrometry (GC-MS). Recoveries on a spiked (20 and 200 µg kg −1 ) sediment ranged from 80% to 91% with calculated limits of detection of 1−5 µg kg −1 dry weight sediment. An additional 20 sediment samples were collected in watersheds from the Southeastern United States where chlorothalonil is used widely on peanuts and other crops. None of the target compounds were detected. Laboratory fortified recoveries of chlorothalonil and its degradates in these environmental sediment samples ranged from 75% to 89%.

Journal of Agricultural and Food Chemistry↗

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↗

USGS1990

Production of sulfur gases and carbon dioxide by synthetic weathering of crushed drill cores from the Santa Cruz porphyry copper deposit near Casa Grande, Pinal County, Arizona

Samples of ground drill cores from the southern part of the Santa Cruz porphyry copper deposit, Casa Grande, Arizona, were oxidized in simulated weathering experiments. The samples were also separated into various mineral fractions and analyzed for contents of metals and sulfide minerals. The principal sulfide mineral present was pyrite. Gases produced in the weathering experiments were measured by gas chromatography. Carbon dioxide, oxygen, carbonyl sulfide, sulfur dioxide and carbon disulfide were found in the gases; no hydrogen sulfide, organic sulfides, or mercaptans were detected. Oxygen concentration was very important for production of the volatiles measured; in general, oxygen concentration was more important to gas production than were metallic element content, sulfide mineral content, or mineral fraction (oxide or sulfide) of the sample. The various volatile species also appeared to be interactive; some of the volatiles measured may have been formed through gas reactions.

Journal of Geochemical Exploration↗

USGS2007

Semipermeable membrane devices used to estimate bioconcentration of polychlorinated biphenyls

ABSTRACT: Aquatic organisms passively accumulate hydrophobic organic compounds, such as polychlorinated biphenyls, even when ambient water concentrations of the contaminant are below analytical detection limits. However, contaminant concentrations in tissue samples are subject to an inherently high level of variability due to differences in species, life stage, and gender bioconcentration potentials. Semipermeable membrane devices (SPMDs) were used to sample Aroclor 1254, a mixture of readily bioconcentrated polychlorinated biphenyls (PCBs), in a contaminated wetland near Flat Top, WV. The devices consisted of triolein, a lipid found in fish, enclosed in a polyethylene membrane. SPMDs were deployed in the water column and in direct contact with wetland sediments along a previously identified concentration gradient of PCBs. The devices were retrieved after a 25-day exposure period. Analytes were recovered by dialyzing the devices in nanograde hexane. Hexane dialysates were condensed and analyzed by gas chromatography. All deployed devices sequestered quantifiable amounts of Aroclor 1254. Water-column SPMDs accumulated PCBs far in excess of ambient water concentrations. The devices contacting sediments accumulated PCBs at all sites, though accumulated concentrations did not exceed concentrations in sediment. Patterns of PCB concentration in the devices corresponded to the identified gradient at the site. Results from the water-column SPMDs were used to estimate the concentration of the dissolved, bioavailable fraction of PCBs present in the water column. These concentrations ranged from 0.01 to 0.09 μg/L of bioavailable Aroclor 1254.

Journal of the American Water Resources Associatio↗

USGS2020

Identification of polychlorinated biphenyls in two bald eagles by combined gas-liquid chromatography-mass spectrometry

Polychlorinated biphenyls are widely used industrial compounds marketed in the United States under the trade name Aroclor. They have appeared in fish and wildlife tissues in this country and Europe. They are known to be toxic, but more importantly, their presence in samples along with the commonly occurring organochlorine pesticides complicates the analysis to a serious degree, making identification of pesticide residues by GLC without preliminary separation extremely unreliable. Residues of both polychlorinated biphenyls and organochloride pesticides were present in eagle carcasses. Many of the polychlorinated biphenyl components had retention times identical with those of certain organochlorine pesticide residues. Identification was accomplished by preliminary separations on thin layer plates followed by combined GLC- mass spectromtry.

Journal of the Association of Official Analytical ↗

USGS2000

Comparison of enzyme-linked immunosorbent assay and gas chromatography procedures for the detection of cyanazine and metolachlor in surface water samples

Enzyme-linked immunosorbent assay (ELISA) data from surface water reconnaissance were compared to data from samples analyzed by gas chromatography for the pesticide residues cyanazine (2-[[4-chloro-6-(ethylamino)-l,3,5-triazin-2-yl]amino]-2-methylpropanenitrile ) and metolachlor (2-chloro-N-(2-ethyl-6-methylphenyl)-N-(2-methoxy-1-methylethyl)acetamide). When ELISA analyses were duplicated, cyanazine and metolachlor detection was found to have highly reproducible results; adjusted R2s were 0.97 and 0.94, respectively. When ELISA results for cyanazine were regressed against gas chromatography results, the models effectively predicted cyanazine concentrations from ELISA analyses (adjusted R2s ranging from 0.76 to 0.81). The intercepts and slopes for these models were not different from 0 and 1, respectively. This indicates that cyanazine analysis by ELISA is expected to give the same results as analysis by gas chromatography. However, regressing ELISA analyses for metolachlor against gas chromatography data provided more variable results (adjusted R2s ranged from 0.67 to 0.94). Regression models for metolachlor analyses had two of three intercepts that were not different from 0. Slopes for all metolachlor regression models were significantly different from 1. This indicates that as metolachlor concentrations increase, ELISA will over- or under-estimate metolachlor concentration, depending on the method of comparison. ELISA can be effectively used to detect cyanazine and metolachlor in surface water samples. However, when detections of metolachlor have significant consequences or implications it may be necessary to use other analytical methods.

Journal of Agricultural and Food Chemistry↗

USGS2010

Use of volatile organic components in scat to identify canid species

Identification of wildlife species from indirect evidence can be an important part of wildlife management, and conventional +methods can be expensive or have high error rates. We used chemical characterization of the volatile organic constituents (VOCs) in scat as a method to identify 5 species of North American canids from multiple individuals. We sampled vapors of scats in the headspace over a sample using solid-phase microextraction and determined VOC content using gas chromatography with a flame ionization detector. We used linear discriminant analysis to develop models for differentiating species with bootstrapping to estimate accuracy. Our method correcdy classified 82.4% (bootstrapped 95% CI = 68.8-93.8%) of scat samples. Red fox (Vulpes vulpes) scat was most frequendy misclassified (25.0% of scats misclassified); red fox was also the most common destination for misclassified samples. Our findings are the first reported identification of animal species using VOCs in vapor emissions from scat and suggest that identification of wildlife species may be plausible through chemical characterization of vapor emissions of scat.

Journal of Wildlife Management↗

USGS1981

Geochemical prospecting for hydrocarbons in the outer continental shelf, Southern Bering Sea, Alaska

This geochemical survey is based on 20 stations located on the outer continental shelf of the southern Bering Sea in an area of 30,000 km 2 that includes St. George basin. Hydrocarbon gases from sediment samples recovered by gravity coring at each of the stations were analyzed by gas chromatography. Data are summarized for a subbottom depth of 0.5 m, because core penetration, although variable, reached at least this depth at all of these stations. Two parameters were used to distinguish the possible presence of thermogenic hydrocarbons: (1) ratios less than 50 of methane to ethane plus propane; and (2) ratios greater than 1 of ethane to ethene. No major hydrocarbon anomalies were discovered; however, at two stations at the northern end of St. George basin, our data indicate that thermogenic hydrocarbons may be present at depth. Major faulting in the vicinity of these stations could provide the pathways for the gas.

Journal of Geochemical Exploration↗

USGS1995

Concentrations of dissolved and particulate Polychlorinated Biphenyls in water from the Saginaw River, Michigan

The Saginaw River receives water from a major drainage basin in the east-central portion of the lower peninsula of Michigan. Historically the river has been contaminated with polychlorinated biphenyls (PCBs) from several sources. The present study was conducted to determine the concentrations of PCBs in both the dissolved and particulate phases of water in the lower Saginaw River, as well as the relative contribution of PCBs from the lower portion of the river relative to more upstream locations. Water samples were collected in 1990–1991, during a range of discharge conditions. Suspended particulates were collected from water onto glass-fiber filters by use of a “Penta-plate” filtration apparatus. Filtered water was subsequently passed through XAD-2 macroreticular resin to collect the “dissolved” PCBs. Concentrations of PCBs in both phases were determined by congener specific gas chromatography with electron capture detection. Total concentrations of PCBs ranged from 11 to 31 ng/L. The concentrations of PCBs in the dissolved phase ranged from 1.9 to 16 ng/L. The ratio of total PCBs bound to suspended particulates, relative to dissolved PCBs, was 2:1 and remained fairly constant for discharges less than approximately 400 M 3 /sec. The loading of total PCBs to Saginaw Bay was estimated to be 225 kg/yr, of which approximately 60% was found to be contributed by the lower 8 km of the Saginaw River.

Michigan↗

USGS2020

Determination of low concentrations of acetochlor in water by automated solid-phase extraction and gas chromatography with mass-selective detection

A sensitive and reliable gas chromatographic/mass spectrometric (GC/MS) method for determining acetochlor in environmental water samples was developed. The method involves automated extraction of the herbicide from a filtered 1 L water sample through a C 18 solid-phase extraction column, elution from the column with hexane-isopropyl alcohol (3 + 1), and concentration of the extract with nitrogen gas. The herbicide is quantitated by capillary/column GC/MS with selected-ion monitoring of 3 characteristic ions. The single-operator method detection limit for reagent water samples is 0.0015 μg/L Mean recoveries ranged from about 92 to 115% for 3 water matrixes fortified at 0.05 and 0.5 μg\L. Average single-operator precision, over the course of 1 week, was better than 5%.

Journal of AOAC International↗

USGS1992

Synthetic organic agrochemicals in the lower Mississippi River and its major tributaries--Distribution, transport and fate

The Mississippi River and its major tributaries transport herbicides and their degradation products from agricultural areas in the mid-western U.S.A. These compounds include atrazine and its degradation products (desethyl- and desisopropylatrazine), simazine, cyanazine, metolachlor, and alachlor and its degradation products (2-chloro-2′,6′-diethylacetanilide 2-hydroxy-2′,6′-diethylacetanilide and 2,6-diethylaniline). These compounds were identified and confirmed by gas chromatography-ion trap mass spectrometry. Loads of these compounds were determined during five sampling trips in 1987–1989. Stream loads of these compounds indicated that atrazine and metolachlor were relatively conservative in downstream transport. Alachlor and its degradation products were generated from point and non-point sources. Seasonal variations and hydrologic conditions controlled the loads of these compounds in the Mississippi River. Cross-channel mixing was slow downstream from major river confluences, possibly requiring several hundred kilometers of downriver transit for completion. The annual transport of these compounds into the Gulf of Mexico was estimated to be < 2% of the annual application of each herbicide in the Midwest.

Journal of Contaminant Hydrology↗