Solid phase extraction gas chromatography/electron capture detector method for the determination of organochlorine pesticides in wildlife whole blood.

A gas chromatographic method for the analysis of 10 organochlorine pesticides in 0.5 mL of whole blood is described. Sample preparation involved an ethyl ether and hexane extraction, followed by a silica solid phase extraction cleanup. The pesticides are quantified by gas chromatography/electron capture detection. Method limits of detection ranged from 1.1 to 5.2 microg/L. The mean and standard deviation for the recovery of 10 pesticides was 97.9 +/- 5.5%. Recoveries from whole blood were comparable to recoveries from plasma. This indicates that the preparation of plasma is unnecessary for the quantification of organochlorine pesticides in blood. This approach is particularly useful as a nonlethal approach for monitoring pesticide contamination in small animals for which the volume of blood is limiting.

Stabilization of the avicide 3-chloro-p-toluidine as the beta-cyclodextrin adduct.

Stabilization of the avicide 3-chloro-p-toluidine (CPTH) on rice baits by pseudo latex polymeric coating and beta-cyclodextin inclusion was investigated. When CPTH-treated rice baits were exposed to sunlight, the CPTH formed colored compounds, which exacerbated problems with bait acceptance and efficacy. Fluidized bed coating with controlled-release polymeric psuedo latexes (RS, RL, NE) reduced CPTH loss but did not eliminate color formation. Enteric pseudo latex coatings (CAP and 4110) gave mixed results. Coating 4110 reduced CPTH loss but still allowed color formation, whereas CAP allowed more CPTH loss than any other coating as well as increased color formation. Inclusion in beta-cyclodextrin (molar ratio 1:1) led to enhanced retention of CPTH and minimal color formation. The CPT/beta-cyclodextrin adduct increased retention of CPTH from 43 to 70% upon simulated weathering. The retention was independent of the adhesives used for attachment.

Determination of propionylpromazine hydrochloride in formulation matrixes using reversed-phase ion-pair small bore liquid chromatography.

Propionylpromazine hydrochloride (PPZHCl) has been investigated for use with leghold traps to reduce the amount of self-inflicted trauma experienced by animals restrained by these traps. Three types of PPZHCl formulations made with Karo dark syrup, K-Y Jelly, and Vaseline were used in 2 types of tranquilizer trap devices (TTDs). A reversed-phase ion-pair liquid chromatography (LC) method using a small bore C18 column was used to: (1) determine the purity of the PPZHCl material used in these formulations, and (2) to determine the resulting PPZHCl content of each formulation. Analyte quantitation was done using UV absorption at 280 nm. Regression analysis of calibration standard solutions indicated a linear and directly proportional relationship between analyte response and PPZHCl concentration over the range evaluated. Recovery data from: (1) Vaseline formulations containing 38.8, 16.2, and 8.78% PPZHCl were 104, 92.9, and 90.2%, respectively, (2) Karo dark syrup formulations containing 26.5, 18.1, and 10.3% PPZHCl were 97.7, 99.3, and 106%, respectively, and (3) K-Y Jelly formulations containing 33.0, 23.5, and 13.4% PPZHCl were 100, 99.4, and 88.7%, respectively. The relative standard deviation (RSD) values from triplicate analysis of these formulations ranged from 0.7 to 6.7%. The PPZHCl content from 9 manufactured TTDs, 3 for each formulation type, were analyzed in triplicate and produced RSD values ranging from 0.7-6.8%. These results indicate that the formulation extraction presented could be used to evaluate the PPZHCl content in TTDs prior to field use. The use of a small bore LC column reduced the amount of solvents consumed and hazardous waste generated, compared to sample analysis that uses a more conventional analytical LC column.

Quantitation of pyrethrum residues in brown tree snakes.

A reversed-phase solid-phase extraction-gas chromatography (SPE-GC)-electron capture detection method is developed to quantitate individual rethrin residues in pyrethrum-exposed brown tree snakes. Aliquots (6 g) of homogenized snake tissue are extracted with 10 mL acetonitrile. The rethrins are recovered from the acetonitrile extract and concentrated using C8 SPE. The rethrins are eluted from the SPE column with pentane, evaporated to near dryness, and reconstituted to 1 mL with 1-propanol. Individual rethrins are quantitated using GC analysis of the 1-propanol solution. Method limits of detection for rethrins range from 0.63 to 6.51 ng/g. The mean recovery for all rethrins is 70.8% with a standard deviation of 5.7%. This method is used to successfully quantitate incurred rethrin residues in pyrethrum-exposed brown tree snakes.

Reversed-phase ion-pair liquid chromatographic determination of chlorophacinone and diphacinone in steam-rolled oat baits and steam-rolled oat/wax baits.

A reversed-phase ion-pair liquid chromatographic (LC) method was developed for analysis of steam-rolled oat (SRO) baits fortified with either chlorophacinone or diphacinone. Baits were prepared with and without paraffin wax. Chlorophacinone or diphacinone was extracted from wax-free SRO baits with 5 mM tetrabutylammonium phosphate methanolic ion-pairing solution. Wax baits were initially extracted with petroleum ether and then cleaned up by liquid extraction into methanolic ion-pairing solution containing 20% water. SRO extracts were analyzed with reversed-phase ion-pair LC. Chlorophacinone and diphacinone were quantified by UV absorption at 325 nm. Recoveries from SRO fortified with chlorophacinone at 25 and 150 micrograms/g were 90.7 and 90.8%, respectively, whereas for diphacinone at the same levels, recoveries were 93.5 and 92.3%, respectively. Recoveries from wax baits fortified at 25 and 75 micrograms/g chlorophacinone were 98.5 and 100%, respectively, whereas for diphacinone at the same levels, recoveries were 93.6 and 98.0%, respectively. Method limits of detection for chlorophacinone and diphacinone in SRO baits were estimated to be 1.0 and 0.76 micrograms/g, respectively. Method limits of detection for chlorophacinone and diphacinone in wax baits were estimated to be 4.2 and 2.8 micrograms/g, respectively.

Solid-phase extraction method for the quantitative analysis of organochlorine pesticides in wildlife urine.

A gas chromatographic method for the analysis of nine organochlorine pesticides in wildlife urine is described. Reversed-phase solid-phase extraction is utilized to extract the organochlorine pesticides from urine. The pesticides are recovered by elution with hexane-ethyl ether (1:1) and quantified by gas chromatography with electron-capture detection. Method detection limits range from 1.4 to 2.7 micrograms/L. Mean recoveries for all pesticides are 90.6%.