Gas-Liquid Chromatographic Analysis and Chemical Confirmation of Azodrin (Monocrotophos) Residues in Strawberries

1976 ◽  
Vol 59 (3) ◽  
pp. 637-640
Author(s):  
James F Lawrence ◽  
Harry A McLeod
Keyword(s):  
Detection Limit ◽  
Chromatographic Analysis ◽  
Small Volume ◽  
Anhydrous Sodium Sulfate ◽  
Methylene Chloride ◽  
Photometric Detection ◽  
Flame Photometric Detection ◽  
Fresh Frozen ◽  
Liquid Chromatographic Analysis ◽  
Liquid Chromatographic

Abstract A gas-liquid chromatographic (GLC) method is described for the analysis and confirmation of azodrin (monocrotophos, 3-(dimethoxyphosphinyl)-N-methyl-cis-crotonamide) residues in strawberries. The strawberries are extracted with acetone, and the filtrate is partitioned with a mixture of methylene chloride and petroleum ether followed by further extraction with methylene chloride. The organic phases are combined, dried with anhydrous sodium sulfate, and concentrated to a small volume for GLC analysis on a 3% OV-210 column with flame photometric detection. Identity of the compound is confirmed by chromatography on the same column after trifluoroacetylation of an aliquot of the strawberry extract. The detection limit is about 2 ppb. The types of strawberry samples analyzed were fresh, frozen, pureed, and jam.

Albendazole-Related Drug Residues in Milk and Their Fate during Cheesemaking, Ripening, and Storage

1998 ◽  
Vol 61 (11) ◽  
pp. 1484-1488 ◽  
Author(s):  
DIMITRIOS J. FLETOURIS ◽  
NICKOS A. BOTSOGLOU ◽  
IOANNIS E. PSOMAS ◽  
ANTONIOS I. MANTIS
Keyword(s):  
Detection Limit ◽  
Chromatographic Analysis ◽  
Ion Pair ◽  
Albendazole Sulfoxide ◽  
Albendazole Sulfone ◽  
Related Drug ◽  
Liquid Chromatographic Analysis ◽  
Residue Levels ◽  
Liquid Chromatographic ◽  
And Storage

The level and nature of the albendazole residues in milk of treated cows were determined as a function of the time of milking (12-h intervals), and the fate of those residues during cheesemaking, ripening, and storage was examined when the obtained milk was used for making Teleme cheese. Ion-pair liquid chromatographic analysis with fluorescence detection showed that the albendazole sulfoxide metabolite reached its maximum (523 ± 199 μg/kg) at the lst milking and declined below the detection limit by the 4th milking. The sulfone metabolite attained its highest level (812 ± 99 μg/kg) more slowly (at the 2nd milking) and declined below detection limit by the 13th milking. The 2-aminosulfone metabolite, which was present in the milk obtained at the lst milking, reached its maximum (128 ± 36 μg/kg) at the 3rd milking, and slowly declined to a level below detection limit by the 15th milking. Whey and cheese analysis revealed that about 70% of each major metabolite initially present in milk could be distributed in the whey. The remaining 30% occurred in the cheese at residue levels higher than those initially present in the milk of the 1st or 2nd milking (688 versus 445 or 450 versus 230 μg/kg for albendazole sulfoxide; 890 versus 608 or 1502 versus 783 μg/kg for albendazole sulfone; 19 versus 15 or 161 versus 105 μg/kg for albendazole 2-aminosulfone). Ripening and storage of the cheeses made from milks from the lst or 2nd milkings results in a decrease of the sulfoxide metabolite (to 225 or 206 μg/kg), an increase of the sulfone metabolite (to 1,181 or 1,893 μg/kg), and no effect on the 2-aminosulfone metabolite.

scholarly journals Collection and Analysis of Butyltin Compounds in Air at Nanogram-Per-Cubic-Meter Levels

1996 ◽  
Vol 79 (1) ◽  
pp. 170-174 ◽  
Author(s):  
Kamal Swami ◽  
Rajinder S Narang
Keyword(s):  
Gas Chromatography ◽  
Detection Limit ◽  
Sodium Borohydride ◽  
Analytical Method ◽  
Capillary Gas Chromatography ◽  
Methylene Chloride ◽  
Photometric Detection ◽  
Flame Photometric Detection ◽  
Butyltin Compounds

Abstract An analytical method for determining butyltin chlo rides in air at low nanogram-per-cubic-meter levels was developed. Butyltin chlorides investigated were mono-n-butyltin trichloride (MBTC),di-n-butyltin dichloride (DBTC), and tri-n-butyltin chlo ride (TBTC). These tin chlorides were trapped on cartridges packed with Porapak-N, eluted with methylene chloride containing 0.3% HCI, hy dridized with sodium borohydride, and analyzed by capillary gas chromatography with flame photometric detection. On the basis of a 20 m3 sample, a detection limit of 0.05 ng/m3 can be achieved.

Rapid Liquid Chromatographic Determination of Dimetridazole and Ipronidazole in Swine Feed

1987 ◽  
Vol 70 (4) ◽  
pp. 626-630 ◽  
Author(s):  
Jose E Roybal ◽  
Robert K Munns ◽  
Jeffrey A Hurlbut ◽  
Wilbert Shimoda ◽  
Thomas R Morrison ◽  
...  
Keyword(s):  
Chromatographic Analysis ◽  
Methylene Chloride ◽  
Drug Level ◽  
Chromatographic Determination ◽  
Acid Base ◽  
Liquid Chromatographic Analysis ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic ◽  
Ppm Level

Abstract A simple and rapid method is described for the determination of dimetridazole (DMZ) and ipronidazole (IPR) in swine feeds at various levels (0.11-110 ppm). The drugs are released from feed by prewetting with a buffer, followed by extraction with either methanol or methylene chloride, depending on the drug level; if necessary, an acid-base cleanup is used before the liquid chromatographic analysis. The analytes are separated on a C18 column and monitored at 320 nm for detection and quantitation. Recoveries of DMZ from several feed formulations averaged 108% at the 92.8 ppm level with a standard deviation (SD) of 4.00% and a coefficient of variation (CV) of 3.70%, 101% at the 11.2 ppm level with an SD of 11.9% and a CV of 11.8%, and 100% at the 0.112 ppm level with an SD of 9.27% and a CV of 9.25%. Recoveries of IPR averaged 77.1% at the 12.9 ppm level with an SD of 1.75% and a CV of 2.27%; IPR recoveries averaged 35.2% at the 0.129 ppm level with an SD of 3.39% and a CV of 9.63%.

Liquid-chromatographic analysis for esmolol and its major metabolite in urine.

1986 ◽  
Vol 32 (2) ◽  
pp. 374-376 ◽  
Author(s):  
R Achari ◽  
D Drissel ◽  
J D Hulse
Keyword(s):  
Chromatographic Analysis ◽  
Chromatographic Method ◽  
Methylene Chloride ◽  
Major Metabolite ◽  
Polar Metabolite ◽  
Ultraviolet Absorbance ◽  
Liquid Chromatographic Method ◽  
Liquid Chromatographic Analysis ◽  
Liquid Chromatographic

Abstract We describe a simple, reproducible liquid-chromatographic method for determination of esmolol (a short-acting beta blocker) and its major metabolite in human urine. Esmolol is extracted from urine at a pH of 8.4 into methylene chloride; the more polar metabolite remains in the aqueous phase. We then measure esmolol with a muBondapak C18 column and measure ultraviolet absorbance at 229 nm; the metabolite is analyzed with a Spherisorb phenyl column, with absorbance measured at 280 nm. The average extraction recoveries of esmolol and the metabolite were 95 and 92%, respectively. Standard curves were linear and reproducible for esmolol from 0.025 to 5 mg/L and for the metabolite from 1 to 250 mg/L. Within-day CVs for both compounds were less than 6%.

Determination of Ethylene Oxide and Ethylene Chlorohydrin in Plastic and Rubber Surgical Equipment Sterilized with Ethylene Oxide

1970 ◽  
Vol 53 (2) ◽  
pp. 263-267
Author(s):  
Daniel J Brown
Keyword(s):  
Detection Limit ◽  
Ethylene Oxide ◽  
Chromatographic Analysis ◽  
Ethylene Chlorohydrin ◽  
Surgical Equipment ◽  
Lower Detection Limit ◽  
Lower Detection ◽  
Liquid Chromatographic Analysis ◽  
Liquid Chromatographic

Abstract A method is presented for the determination of ethylene chlorohydrin and ethylene oxide residues in plastic and rubber surgical equipment. Samples are extracted with p-xylene and the desired constituents are isolated by column chromatography. Ethylene oxide is converted to ethylene chlorohydrin on a Celite column. Sweep co-distillation is then employed for further purification, if necessary, before gas-liquid chromatographic analysis. The lower detection limit is approximately 25 ng. Recoveries of 3.5’50 ppm chlorohydrin from 20’35 g samples range from 64 to 100%, depending on the absorbing capacity of the material being analyzed and the condition of the adsorbent.

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