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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↗

USGS2009

Gas chromatographic–mass spectrometric fragmentation study of phytoestrogens as their trimethylsilyl derivatives: Identification in soy milk and wastewater samples

An analytical method for the identification of eight plant phytoestrogens (biochanin A, coumestrol, daidzein, equol, formononetin, glycitein, genistein and prunetin) in soy products and wastewater samples was developed using gas chromatography coupled with ion trap mass spectrometry (GC/MS–MS). The phytoestrogens were derivatized as their trimethylsilyl ethers with trimethylchlorosilane (TMCS) and N,O- bis (trimethylsilyl)trifluoroacetamide (BSTFA). The phytoestrogens were isolated from all samples with liquid–liquid extraction using ethyl acetate. Daidzein-d 4 and genistein-d 4 labeled standards were used as internal standards before extraction and derivatization. The fragmentation patterns of the phytoestrogens were investigated by isolating and fragmenting the precursor ions in the ion-trap and a typical fragmentation involved the loss of a methyl and a carbonyl group. Two characteristic fragment ions for each analyte were chosen for identification and confirmation. The developed methodology was applied to the identification and confirmation of phytoestrogens in soy milk, in wastewater effluent from a soy-milk processing plant, and in wastewater (influent and effluent) from a treatment plant. Detected concentrations of genistein ranged from 50,000 μg/L and 2000 μg/L in soy milk and in wastewater from a soy-plant, respectively, to 20 μg/L and <1 μg/L for influent and effluent from a wastewater treatment plant, respectively.

Journal of Chromatography A↗

USGS2002

Accurate mass analysis of ethanesulfonic acid degradates of acetochlor and alachlor using high-performance liquid chromatography and time-of-flight mass spectrometry

Degradates of acetochlor and alachlor (ethanesulfonic acids, ESAs) were analyzed in both standards and in a groundwater sample using high-performance liquid chromatography–time-of-flight mass spectrometry with electrospray ionization. The negative pseudomolecular ion of the secondary amide of acetochlor ESA and alachlor ESA gave average masses of 256.0750±0.0049 amu and 270.0786±0.0064 amu respectively. Acetochlor and alachlor ESA gave similar masses of 314.1098±0.0061 amu and 314.1153±0.0048 amu; however, they could not be distinguished by accurate mass because they have the same empirical formula. On the other hand, they may be distinguished using positive-ion electrospray because of different fragmentation spectra, which did not occur using negative-ion electrospray.

Journal of Chromatography A↗

USGS2020

American eels produce and release bile acids that vary across life stage

The American eel ( Anguilla rostrata ) is an imperilled fish hypothesized to use conspecific cues, in part, to coordinate long‐distance migration during their multistage life history. Here, holding water and tissue from multiple American eel life stages was collected and analysed for the presence, profile and concentration of bile acids. Distinct bile acid profiles were identified in glass, elver, yellow eel and silver eel holding waters using ultraperformance liquid chromatography high‐resolution mass spectrometry and principal component analysis. Taurochenodeoxycholic acid, taurodeoxycholic acid, cholic acid, deoxycholic acid, taurolithocholic acid and taurocholic acid were detected in whole tissue of American glass eels and elvers, and in liver, intestine and gallbladder samples of late‐stage yellow eels. Bile acids were not a major component of silver eel washings or tissue. This study is novel because little was previously known about bile acids produced and emitted into the environment by American eels. Future behavioural studies could evaluate whether any bile acids produced by American eels influence conspecific migratory behaviour.

Journal of Fish Biology↗

USGS2003

Determination of alkylphenol and alkylphenolethoxylates in biota by liquid chromatography with detection by tandem mass spectrometry and fluorescence spectroscopy

A quantitative method for the simultaneous determination of octylphenol, nonylphenol and the corresponding ethoxylates (1 to 5) in biota is presented. Extraction methods were developed for egg and fish matrices based on accelerated solvent extraction followed by a solid-phase extraction cleanup, using octadecylsilica or aminopropyl cartridges. Identification and quantitation were accomplished by liquid chromatography-electrospray tandem mass spectrometry (LC-MS-MS) and compared to the traditional liquid chromatography with fluorescence spectroscopy detection. LC-MS-MS provides high sensitivity and specificity required for these complex matrices and an accurate quantitation with the use of 13C-labeled internal standards. Quantitation limits by LC-MS-MS ranged from 4 to 12 ng/g in eggs, and from 6 to 22 ng/g in fish samples. These methods were successfully applied to osprey eggs from the Chesapeake Bay and fish from the Great Lakes area. Total levels found in osprey egg samples were up to 18 ng/g wet mass and as high as 8.2 ug/g wet mass in the fish samples.

Journal of Chromatography A↗

USGS1987

Chiral-phase high-performance liquid chromatography of rotenoid racemates

The high-performance liquid chromatograhic (HPLC) behavior of parent rotenoids (type I) and the hydroxyl-analogues (type II) on three different chiral stationary phases (CSPs) was studied. Separations of optical isomers were achieved in various degrees depending largely upon the rotenoidal structures and the CSP types employed. Enantiomers of all but elliptone compounds were separable on β-cyclodextrin-bonded silica (CDS). Without exception, the 12a-hydroxyrotenoid antipodes were resolved on Pirkle's phenylglycine-bonded silica (PGS) despite unsuccessful attenmpts to resolve the type I rotenoidal racemates. Conversely, optical resolution of the latter rotenoids was accomplished by using a helical polytriphenylmethylacrylate-coated silica (TPS) column and the observed separation factors (α values) ranged from 1.14 to 1.90. The results from HPLC of type II rotenoids on TPS (α = 1.00–1.63) suggested that variations in E-ring structures had profound influence on the resolution outcome. Conjugated double bonds on the E-ring and the desisopropylation of the five-membered E-ring ot type II rotenoids appeared to be important structural features for chiral recognition involving the TPS substrate. In both reversed-phase (CDS) and normal-pahse (PGS and TPS) HPLC modes, the less polar enantiomers were the 6aβ,12aβ-rotenoids as observed in most cases, though this relationship was reversed in the cases of deguelin and hydroxyelliptone probably due to conformational effects of rotenoidal ring systems.

Journal of Chromatography↗

USGS1982

High-performance liquid chromatographic resolution and quantification of a dilacton antibiotic mixture (antimycin A)

High-performance liquid chromatographic (HPLC) conditions are presented for the separation and quantitative determination of a homologous antibiotic complex (antimycin A). Combined HPLC and chemical ionization mass spectrometry proved to be exceptionally useful for the structural identification of chromatographic components. Using electrochemical, fluorescence, and ultraviolet detectors, the minimum detectable amounts of the antibiotics were found to be in the ranges 0.10–1.12, 0.31–1.69, and 4.10–28.2 ng, respectively. Advantages of the preparation of Dns derivatives for use in fluorescence detection are discussed. Application of the HPLC technique to the analysis of the antibiotic mixture in organic tissues is demonstrated.

Journal of Chromatography↗

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↗

USGS2002

Analysis and detection of the herbicides dimethenamid and flufenacet and their sulfonic and oxanilic acid degradates in natural water

Dimethenamid [2-chloro-N-(2,4-dimethyl-3-thienyl)-N-(2-methoxy-1-methylethyl)acetamide] and flufenacet [N-(4-fluorophenyl)-N-(1-methylethyl)-2-(5-(trifluoromethyl)-1,3,4- thiadiazol-2-yl)oxy] were isolated by C-18 solid-phase extraction and separated from their ethanesulfonic acid (ESA) and oxanilic acid (OXA) degradates during their elution using ethyl acetate for the parent compound, followed by methanol for the polar degradates. The parent compounds were detected using gas chromatography-mass spectrometry in selected-ion mode. The ESA and OXA degradates were detected using high-performance liquid chromatography-electrospray mass spectrometry (HPLC-ESPMS) in negative-ion mode. The method detection limits for a 123-mL sample ranged from 0.01 to 0.07 μg/L. These methods are compatible with existing methods and thus allow for analysis of 17 commonly used herbicides and 18 of their degradation compounds with one extraction. In a study of herbicide transport near the mouth of the Mississippi River during 1999 and 2000, dimethenamid and its ESA and OXA degradates were detected in surface water samples during the annual spring flushes. For flufenacet, the only detections at the study site were for the ESA degradates in samples collected at the peak of the herbicide spring flush in 2000. The low frequency of detections in surface water likely is due to dimethenamid and flufenacet being relatively new herbicides. In addition, detectable amounts of the stable degradates have not been detected in ground water.

Journal of Agricultural and Food Chemistry↗

USGS1982

A rapid high-performance liquid-chromatographic method for simultaneously determining the concentrations of TFM and Bayer 73 in water during lampricide treatments

The high-performance liquid-chromatography (HPLC) procedure requires only minutes per sample, is specific, and is relatively sensitive (limit of detection < 0.005 mg/L for both chemicals). A combined buffer (pH 4) and internal standard (3-chlorodiphenylamine) reagent is added to the water sample, which is injected through a Sep Pak C 18 disposable cartridge. The cartridge adsorbs and retains both the lampricides and the internal standard. The quantitative elution of the three chemicals from the cartridge with a small volume of methanol effectively concentrates the sample and provides sample cleanup. The methanol extract is then analyzed directly by HPLC on an MCH 10 reverse phase column by using a methanol:0.01 mol/L acetate buffer (87:13, v:v) as the mobile phase at 2 mL/min and detected by ultraviolet spectrophotometry at 330 (or 254) nm. A microprocessor data system further facilitates the procedure by quantifying off-scale peaks and yielding results directly in units of concentration (mg/L).

Canadian Journal of Fisheries and Aquatic Sciences↗

USGS2002

Determination of vapor pressures for nonpolar and semipolar organic compounds from gas chromatographic retention data

Vapor pressures for nonpolar and moderately polar organochlorine, pyrethroid, and organophosphate insecticides, phthalate esters, and organophosphate flame retardants were determined by capillary gas chromatography (GC). Organochlorines and polycyclic aromatic hydrocarbons with known liquid-phase vapor pressures (P??L) (standard compounds) were chromatographed along with two reference compounds n-C20 (elcosane) and p,p???-DDT on a 1.0-m-long poly(dimethylsiloxane) bonded-phase (BP-1) column to determine their vapor pressures by GC (P??GC). A plot of log P??L vs log P??GC for standard compounds was made to establish a correlation between measured and literature values, and this correlation was then used to compute P??L of test compounds from their measured P??GC. P??L of seven major components of technical chlordane, endosulfan and its metabolites, ??-hexachlorocyclohexane, mirex, and two components of technical toxaphene were determined by GC. This method provides vapor pressures within a factor of 2 of average literature values for nonpolar compounds, similar to reported interlaboratory precisions of vapor pressure determinations. GC tends to overestimate vapor pressures of moderately polar compounds. ?? 1990 American Chemical Society.

Journal of Chemical and Engineering Data↗

USGS1991

Rotenone persistence in freshwater ponds: Effects of temperature and sediment adsorption

The persistence of rotenone was compared between a cement-lined pond (0.04 hectare) and an earthen-bottom pond (0.02 hectare) treated with 5 μL Noxfish/L (250 μg rotenone/L) during spring, summer, and fall. Water temperatures on the days of treatment in each season were 8, 22, and 15°C, respectively. Both ponds were filled with pond water from a common source 1 week before each of the three treatments. Water samples (filtered and unfiltered) and sediment samples were analyzed by high-performance liquid chromatography to monitor the decrease of rotenone until residues were at or below the detection limit (<2.0 μg/L for water and < 25 ng/g for sediments). The loss of rotenone from water generally followed a first-order rate ofdecay. Rotenone disappeared two to three times faster in the earthen pond than in the concrete pond. The rotenone half-life times in the spring, summer, and fall treatments were 3.7, 1.3, and 5.2 d, respectively, in the concrete pond, and 1.8, 0.7, and 1.8 d in the earthen pond. Rates of decay in both ponds were directly correlated with water temperature. Filtered water samples from both ponds contained less rotenone than unfiltered water, indicating that some rotenone was bound to suspended material. The highest concentration of rotenone in sediment samples was 102 ng/g; residues decreased to below the detection limit within 14 d in the spring treatment and within 3 d in the summer and fall treatments.

North American Journal of Fisheries Management↗

USGS2010

Effect of diet on fecal and urinary estrogenic activity

The United States Environmental Protection Agency has identified estrogens from animal feeding operations as a major environmental concern, but few data are available to quantify the excretion of estrogenic compounds by dairy cattle. The objectives of this study were to quantify variation in estrogenic activity in feces and urine due to increased dietary inclusion of phytoestrogens. Ten Holstein heifers were assigned to 2 groups balanced for age and days pregnant; groups were randomly assigned to treatment sequence in a 2-period crossover design. Dietary treatments consisted of grass hay or red clover hay, and necessary supplements. Total collection allowed for sampling of feed refusals, feces, and urine during the last 4 d of each period. Feces and urine samples were pooled by heifer and period, and base extracts were analyzed for estrogenic activity (estrogen equivalents) using the yeast estrogen screen bioassay. Feces and urine samples collected from 5 heifers were extracted and analyzed using liquid chromatography-tandem mass spectrometry (LC-MS/MS) to quantify excretion of 7 phytoestrogenic compounds. Excretion of 17-β estradiolequivalents in urine was higher and tended to be higher in feces for heifers fed red clover hay (84.4 and 120.2 mg/d for feces and urine, respectively) compared with those fed grasshay (57.4 and 35.6 mg/d). Analysis by LC-MS/MS indicated greater fecal excretion of equol, genistein, daidzein, coumestrol, and formononetin by heifers fed red clover hay (1634, 29.9, 96.3, 27.8, and 163 mg/d, respectively) than heifers fed grass hay (340, 3.0, 46.2, 8.8, and 18.3 mg/d, respectively). Diet had no effect on fecal biochanin A or 2-carbethoxy-5, 7-dihydroxy-4’-methoxyisoflavone. Four phytoestrogens were detected in urine (2-carbethoxy-5, 7-dihydroxy-4’-methoxyisoflavone, daidzein, equol, and formononetin) and their excretion was not affected by diet. Identifying sources of variation in estrogenic activity of manure will aid in the development of practices to reduce environmental estrogen accumulation.

Journal of Dairy Science↗

USGS1983

High-performance liquid chromatography of quinoidal imminium compounds derived from triphenylmethanes

A series of eleven p -aminotriphenylmethane dyes have been studied by high-performance liquid chromatography (HPLC). The combined use of HPLC and spectrophotometry permits specific detection of these compounds in the visible range around 600 nm. As the high affinity of the imminium cations for the active sites of the hydrocarbonaceous stationary phase has presented difficulties for reversed-phase HPLC with pure solvents, organic electrolytes were added to the mobile phase to facilitate the elution of the components with improved selectivity, sensitivity (minimum detection limit, 0.1 μg/ml), and peak symmetry. The effects of chromatographic variables on the component retentivity were investigated. Retention times of the dye analytes decreased with increasing concentration of the added ionic reagent and with decreasing number of the hydrophobic alkyl substituents on the nitrogen atom. The influence of pH on the retention parameters appears to parallel that observed previously for cationic quaternary ammonium compounds. Among the acidic reagents employed, naphthalenesulfonic acid yielded the most satisfactory results. The use of binary electrolyte systems invariably improved the chromatographic behavior of the imminium solutes analyzed. Results obtained with two different octadecylsilica columns have been compared.

Journal of Chromatography↗

USGS1981

Speciation of aryloxyethoxyethyl benzyl dimethyl ammonium salts by glass capillary gas chromatography and high-performance liquid chromatography

Using glass capillary gas chromatography (GC) and ion-pair reversed-phase high-performance liquid chromatography (HPLC), a pair of structurally similar microbicides, benzyl diisobutylphenoxyethoxyethyl dimethyl ammonium chloride and its cresoxy-analogue, were effectively resolved and accurately quantified with a high degree of selectivity and specificity. Optimization of conditions in the chromatographic systems to attain desirable baseline separations of the components of interest is described. The minimum detectable quantities as determined are in the neighborhood of 10 ng for the quaternary ammonium salts by HPLC-UV detection, 0.1 ng for the cyanamide derivatives of the salts by GC-alkaline flame-ionization detection and 1–2 pg for the trichloroethyl carbamate derivatives of the salts by GC-electron-capture detection. In conjunction with cation-exchange chromatography for sample enrichment and purification, the glass capillary GC and ion-pair reversed-phase HPLC methods presented here are particularly suitable to separate and simultaneously analyze for the aryloxyethoxyethyl benzyl dimethyl ammonium compounds concerned in environmental samples. It appears that these chromatographic techniques possess potential applicability to the separation and quantification of other classes of quaternary ammonium compounds with closely related structures that are not separable by other methods.

Journal of Chromatography↗

USGS2014

Pharmacokinetics of hydromorphone hydrochloride after intravenous and intramuscular administration of a single dose to American kestrels (Falco sparverius)

Objective —To determine the pharmacokinetics of hydromorphone hydrochloride after IV and IM administration in American kestrels ( Falco sparverius ). Animals —12 healthy adult American kestrels. Procedures —A single dose of hydromorphone (0.6 mg/kg) was administered IM (pectoral muscles) and IV (right jugular vein); the time between IM and IV administration experiments was 1 month. Blood samples were collected at 5 minutes, 1 hour, and 3 hours (n = 4 birds); 0.25, 1.5, and 9 hours (4); and 0.5, 2, and 6 hours (4) after drug administration. Plasma hydromorphone concentrations were determined by means of liquid chromatography with mass spectrometry, and pharmacokinetic parameters were calculated with a noncompartmental model. Mean plasma hydromorphone concentration for each time was determined with naïve averaged pharmacokinetic analysis. Results —Plasma hydromorphone concentrations were detectable in 2 and 3 birds at 6 hours after IM and IV administration, respectively, but not at 9 hours after administration. The fraction of the hydromorphone dose absorbed after IM administration was 0.75. The maximum observed plasma concentration was 112.1 ng/mL (5 minutes after administration). The terminal half-life was 1.25 and 1.26 hours after IV and IM administration, respectively. Conclusion and Clinical Relevance —Results indicated hydromorphone hydrochloride had high bioavailability and rapid elimination after IM administration, with a short terminal half-life, rapid plasma clearance, and large volume of distribution in American kestrels. Further studies regarding the effects of other doses, other administration routes, constantrate infusions, and slow release formulations on the pharmacokinetics of hydromorphone hydrochloride and its metabolites in American kestrels may be indicated.

American Journal of Veterinary Research↗

USGS2015

Quantification of 15 bile acids in lake charr feces by ultra-high performance liquid chromatography–tandem mass spectrometry

Many fishes are hypothesized to use bile acids (BAs) as chemical cues, yet quantification of BAs in biological samples and the required methods remain limited. Here, we present an UHPLC–MS/MS method for simultaneous, sensitive, and rapid quantification of 15 BAs, including free, taurine, and glycine conjugated BAs, and application of the method to fecal samples from lake charr ( Salvelinus namaycush ). The analytes were separated on a C 18 column with acetonitrile–water (containing 7.5 mM ammonium acetate and 0.1% formic acid) as mobile phase at a flow rate of 0.25 mL/min for 12 min. BAs were monitored with a negative electrospray triple quadrupole mass spectrometer (Xevo TQ-S™). Calibration curves of 15 BAs were linear over the concentration range of 1.00–5,000 ng/mL. Validation revealed that the method was specific, accurate, and precise. The method was applied to quantitative analysis of feces extract of fry lake charr and the food they were eating. The concentrations of analytes CA, TCDCA, TCA, and CDCA were 242.3, 81.2, 60.7, and 36.2 ng/mg, respectively. However, other taurine conjugated BAs, TUDCA, TDCA, and THDCA, were not detected in feces of lake charr. Interestingly, TCA and TCDCA were detected at high concentrations in food pellets, at 71.9 and 38.2 ng/mg, respectively. Application of the method to feces samples from lake charr supported a role of BAs as chemical cues, and will enhance further investigation of BAs as chemical cues in other fish species.

Journal of Chromatography B: Analytical Technologi↗

USGS2008

Environmental occurrence and shallow ground water detection of the antibiotic monensin from dairy farms

Pharmaceuticals used in animal feeding operations have been detected in various environmental settings. There is a growing concern about the impact on terrestrial and aquatic organisms and the development of antibiotic-resistant strains of microorganisms. Pharmaceutical use in milking cows is relatively limited compared with other livestock operations, except for the ionophore monensin, which is given to lactating cows as a feed. By weight, monensin can be the most significant antibiotic used in a dairy farm. This study investigates the potential of monensin to move from dairy operations into the surrounding ground water. Using two dairy farms in California as study sites, we twice collected samples along the environmental pathway-from flush lanes, lagoon waters, and shallow ground water beneath the dairies and beneath its associated manured fields. Monensin concentrations were determined using solid-phase extraction and liquid chromatography-tandem mass spectrometry with positive electrospray ionization. Monensin was detected in all of the flush lane and lagoon water samples. Theoretical maximum concentration estimated from the actual dosing rate and the theoretical excretion rate assuming no attenuation was one order of magnitude greater than observed concentrations, suggesting significant attenuation in the manure collection and storage system. Monensin was also detected, at levels ranging from 0.04 to 0.39 microg L(-1), in some of the ground water samples underneath the production area of the dairy but not from the adjacent manured fields. Concentrations in ground water immediately downgradient of the lagoons were one to two orders of magnitude lower than the concentrations detected in lagoons, suggesting attenuation in the subsurface. The data suggest the possibility of monensin transport into shallow (2-5 m) alluvial ground water from dairy management units, including manure storage lagoons and freestalls occupied by heifers, lactating cows, and dry cows.

Journal of Environmental Quality↗