用液相色谱法测定牛乳中的头孢噻呋
Determination of ceftiofur in bovine milk by liquid chromatography.
作者信息
McNeilly P J, Reeves V B, Deveau E J
机构信息
US Food and Drug Administration, Center for Veterinary Medicine, Agricultural Research Center-East, Beltsville, MD 20705, USA.
出版信息
J AOAC Int. 1996 Jul-Aug;79(4):844-7.
A liquid chromatographic procedure is described for determination of ceftiofur (CEF) residues in milk. Milk samples were diluted with ammonium acetate solution and extracted on a C18 solid-phase extraction (SPE) column. After the analyte was eluted from the SPE column with methanol, extract volumes were reduced under nitrogen, diluted to 2.0 mL with acetate buffer, and filtered. CEF was determined after separation of milk components by reverse-phase chromatography with UV detection at 293 nm. Recoveries of CEF from bovine milk fortified at 25, 50, and 100 ppb were 86.1, 90.8, and 92.0%, respectively, with coefficients of variation (CVs) of 6.4, 7.3, and 3.9%, respectively. Values of CEF obtained from analysis of milk containing 2 levels of biologically incurred residues were 26.1 and 67.3 ppb with CVs of 3.8 and 4.4%, respectively. The limits of detection and quantitation were estimated to be 4 and 7 ppb, respectively.
描述了一种用于测定牛奶中头孢噻呋（CEF）残留量的液相色谱方法。牛奶样品用醋酸铵溶液稀释，并在C18固相萃取（SPE）柱上进行萃取。用甲醇从SPE柱上洗脱分析物后，在氮气下减少萃取液体积，用醋酸盐缓冲液稀释至2.0 mL并过滤。通过反相色谱在293 nm处进行紫外检测，分离牛奶成分后测定CEF。在添加了25、50和100 ppb头孢噻呋的牛奶中，回收率分别为86.1%、90.8%和92.0%，变异系数（CV）分别为6.4%、7.3%和3.9%。对含有2个水平生物源性残留的牛奶进行分析，得到的头孢噻呋值分别为26.1和67.3 ppb，CV分别为3.8%和4.4%。检测限和定量限估计分别为4和7 ppb。
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