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A comparison was made of virus recovery from inoculated glass surfaces by 3 different viral recovery techniques used in spray test methods. On a total of 7, 5, and 5 observations, for the cover glass crushing, cotton swab rubbing, and microscopic slide shaking techniques, respectively, the log reduction of the median tissue culture infective dose (log TCID-50/ml) averaged 1.48, 2.57, and 2.22, the mean percentage recovery was 77.98, 61.55, and 66.94%, and the coefficient of variation was 4.37, 10.01, and 7.42%. The cover glass technique was found to be the least variable and the most effective and precise of the 3 methods.
J Assoc Off Anal Chem 1975 Jan
PMID:Comparison of virus recovery techniques for assessing the virucidal activity of disinfectant spray products. 16 73

Some 10% and lower guarantee carbaryl dusts cannot be quantitatively extracted by shaking with chloroform as specified in the official first action infrared method for carbaryl formulations, 6.206-6.208. A repeatability extraction study has been made, using a different extraction technique with both chloroform and 10% methanol in chloroform. The results indicate that the new extraction technique and the mixed solvent are suitable for all solid carbaryl formulations. It is recommended that a collaborative study be conducted on the new solvent system and extraction technique.
J Assoc Off Anal Chem 1975 Jan
PMID:Carbaryl insecticide: extraction from dust and powder formulations. 80 73

Polarographic residue methods have been developed for determining robenidine (Robenz), 1,3-bis[p-chlorobenzylidene)amino]-guanidine monohydrochloride, in chicken tissues, eggs, litter, soil, and plants. The compound is extracted from chicken fat, skin, muscle, liver, and eggs with ethyl acetate; from blood with acetone; from plant tissue, litter, and kidney with acidic acetone; and from soil with basic methanol. After extraction by high-speed blending or overnight shaking, the extract is cleaned up by evaporation, solvent partition and/or elution from CG-50 ion exchange resin. Robenidine is quantitated by differential cathode ray polarography, using acidic aqueous methanol or acetic acid (1+1) supporting electrolyte. Recoveries ranged from 64 to 125% with an average overall recovery of 90%. The validated sensitivity is 0.1 ppm for chicken tissues, soil, and plants, 0.01 ppm for eggs, and 1 ppm for litter.
J Assoc Off Anal Chem 1977 Nov
PMID:Polarographic determination of robenidine residues in chicken tissues, eggs, litter, soil, and plant tissue. 92 34

Mestranol in combination with ethynodiol diacetate, an oral contraceptive formulation, is isolated from the sample on a partition chromatographic column prior to colorimetric determination. The color reaction which is specific for estrogens is formed by shaking an aliquot of the heptane eluate of mestranol with a 30% methanol-sulfuric acid solution. A collaborative study of the method gave results of 99.8% of added mestranol for the simulated mix and 100.7% of labelled mestranol for the commercial tablet. The method has been adopted as official first aciton.
J Assoc Off Anal Chem 1975 Jan
PMID:Colorimetric determination of mestranol in combination with ethynodiol diacetate. 114 Nov 59

A simple and rapid high-performance liquid chromatographic procedure is described for the determination of strychnine. Grain baits containing strychnine alkaloid are ground, mixed, and extracted by shaking with chloroform. Without further cleanup, extract filtrates are injected directly into a liquid chromatograph. Chromatography is complete within 7 min and peak heights are used for quantitation. Separations were made on a 30 cm times 4 mm id stainless steel column packed with mu Porasil (8-12 mum silica). The eluting solvent was methanol-chloroform (10+90) at a flow rate of 2.0 ml/min. Recovery of spiked samples ranged from 91.5 to 95.2%. Confirmation of strychnine from a commercial sample was made by high resolution mass spectrometry with mass agreement to 1.2 ppm.
J Assoc Off Anal Chem 1975 Sep
PMID:High-performance liquid chromatographic determination of strychnine in grain baits.l. 115 38

A simple and rapid gas-liquid chromatographic procedure, using a 6' times 1/4'' glass column packed with 5% SE-30 on Chromosorb W (DMCS) and a flame ionization detector, is described. Grain baits containing strychnine alkaloid are ground, mixed, and extracted by shaking with chloroform containing an internal standard, 1,3,5-triphenylbenzene. Without further cleanup, extract filtrates are injected directly into a gas chromatograph. Peak height ratios are used for quantitation of strychnine. The analysis of commercial samples shows that the method compares well with a commonly employed ultraviolet spectrophotometric method; good precision, with recoveries ranging from 89.9 to 91.7%, is obtained in the analysis of prepared samples. The method is sensitive to 2 mug strychnine.
J Assoc Off Anal Chem 1975 Sep
PMID:Gas-liquid chromatographic determination of strychnine in grain baits. 115 39

Results are compared for the microbiological analysis of chlortetracycline using the AOAC method and a modified method applicable to potencies above 50 g/ton. Two modifications are presented: substitution of a pH range of 4.0-4.5 instead of the specified pH of 4.5 for the plating solution, and substitution of extraction by shaking instead of the blending procedure. There were no significant differences in results between the AOAC method and the modified method.
J Assoc Off Anal Chem
PMID:Modifications to the official method for testing chlortetracycline HCl in animal feeds. 178 87

A rapid liquid chromatographic (LC) method was developed for a sensitive determination of nitrite in cured meats, using ion-exclusion chromatographic separation and electrochemical detection (IEC-EC). The current AOAC colorimetric method requires 2 h shaking in a steam bath to eliminate interference from reducing compounds such as ascorbic acid. In the present method, nitrite was analyzed in the presence of ascorbic acid without interference, and the extraction time was reduced to 1 min. The extracted nitrite was determined by ion chromatography using anion-exclusion/HS column and amperometric detector equipped with platinum or glassy carbon electrode operating at +1.0 V vs Ag/AgCl reference electrode. The detection limit was 1 ppb as NO2-. The recoveries of 50 ppm nitrite added to frankfurter and meat stick were 103 and 99.6%, respectively, with relative standard deviations less than 4%. The high speed, sensitivity, and selectivity make the new method a useful alternative to the AOAC colorimetric method.
J Assoc Off Anal Chem
PMID:Determination of nitrite in cured meats by ion-exclusion chromatography with electrochemical detection. 221 78

A method was developed for extraction of weathered residues of atrazine and metolachlor from field soils; soils had last been treated with commercial formulations of the herbicides 8-15 months prior to sample collection. Maximum yields were obtained by batch extraction at 75 degrees C for 2-16 h with methanol-water (80 + 20) in a sealed vial. Hydrolysis or other decomposition reactions were minor or negligible, depending on the extraction time. This method is an improvement over published methods that are validated by spike recoveries; the proposed method gives 1.7-1.8 times higher yields compared to shaking for 2 h at room temperature, and 1.3-1.8 times higher yields compared to Soxhiet extraction. The reproducibility of the method was better than 12%. The results underscore the impact of nonequilibrium sorption of organic compounds on analytical methodology and emphasize the need to validate extraction methods with field samples.
J Assoc Off Anal Chem
PMID:Improved extraction of atrazine and metolachlor in field soil samples. 237 50

A sensitive method is described to determine trace quantities of ethylene oxide (EO) in EO-sterilized intraocular lenses (IOLs). An IOL is dipped in ethanol containing 0.25 ppm propylene oxide (PO) in a 4 mL vial, 2 drops of freshly distilled hydrobromic acid is added through a septum, and the mixture is warmed at 50 degrees C for 24 h. It is then neutralized by vigorous shaking with sodium bicarbonate, dehydrated with anhydrous sodium sulfate, and filtered. The filtrate is injected into a gas chromatograph with electron-capture detection, and the peak height ratio of ethylene bromohydrin/propylene bromohydrin is measured. EO residue is calculated from the calibration curve obtained through a similar procedure with the standard EO/PO solutions. The limit of determination is 0.04 microgram/lens (ca 2.0 ppm). When EO residue levels were determined for IOLs sampled at 3 different aeration periods after sterilization, we found that 9 days of aeration was necessary to meet the U.S. Food and Drug Administration proposed limit for EO residue in IOLs.
J Assoc Off Anal Chem
PMID:Gas chromatographic determination with electron capture detection of residual ethylene oxide in intraocular lenses. 323 2


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