Simultaneous determination of five fasciolicides in milk by liquid chromatography with electrochemical detection.
A sensitive and specific method is described for determination of 5 fasciolicides in milk. The drugs are used to control liver flukes in cattle. The milk sample was homogenized with acetone and acetonitrile, sonicated, and centrifuged. The supernatant was extracted with dichloromethane. The extract was evaporated to dryness, dissolved in 1% sodium hydrogen carbonate, and purified on a C18 cartridge. The 5 drugs were separated from the matrix by reversed-phase liquid chromatography (LC) and determined by dual-electrode coulometric detection on a Kaseisorb LC ODS-300-5 column. The mobile phase was acetonitrile-0.05M potassium dihydrogen phosphate (55 + 45) at pH 3.0. The flow rate was 1 mL/min at 40 degrees C. The applied potentials of detectors 1 and 2 were set at 0.20 and 0.55 V, respectively. The average recovery of the drugs added to milk at 0.01 and 0.1 micrograms/mL was 89.6%, and the coefficient of variation was 4.7%. The detection limits of the drugs in milk were 4-20 ng/mL. The method is used to monitor commercial milk samples and to determine the residual levels of these drugs in milk from cows treated with a fasciolicide.
Takeba
K
K
Tokyo Metropolitan Research Laboratory of Public Health, Department of Food Hygiene and Nutrition, Japan.
Itoh
T
T
Matsumoto
M
M
Nakazawa
H
H
Tanabe
S
S
D000096:Acetone / Q000737:chemistry; D000097:Acetonitriles / Q000737:chemistry; D000818:Animals; D000871:Anthelmintics / Q000032:analysis* / Q000378:metabolism; D001735:Bithionol / Q000032:analysis / Q000378:metabolism; D002417:Cattle; D002733:Chlorophenols / Q000032:analysis / Q000378:metabolism; D002851:Chromatography, High Pressure Liquid; D002853:Chromatography, Liquid; D004350:Drug Residues / Q000032:analysis* / Q000378:metabolism; D004563:Electrochemistry; D008401:Gas Chromatography-Mass Spectrometry; D008892:Milk / Q000737:chemistry* / Q000378:metabolism; D010097:Oxyclozanide / Q000032:analysis / Q000378:metabolism; D011075:Polybrominated Biphenyls / Q000032:analysis / Q000378:metabolism; D012015:Reference Standards; D012458:Salicylanilides / Q000032:analysis / Q000378:metabolism; D012680:Sensitivity and Specificity; D017693:Sodium Bicarbonate / Q000737:chemistry
D000097:Acetonitriles; D000871:Anthelmintics; D002733:Chlorophenols; D011075:Polybrominated Biphenyls; D012458:Salicylanilides; D000096:Acetone; D010097:Oxyclozanide; C004361:tribromsalan; C036629:oxynide; D017693:Sodium Bicarbonate; D001735:Bithionol; C018474:bromophenophos; C032159:acetonitrile