Cox B L, Krzeminski L F
J Assoc Off Anal Chem. 1982 Nov;65(6):1311-5.
A high pressure liquid chromatographic (HPLC) method has been developed for determination of sulfamethazine residues in pork liver, kidney, muscle, and fat. The sample was extracted with acetone-chloroform, concentrated in the presence of dilute HCl, and partitioned between dilute HCl and hexane. The acid solution was washed with methylene chloride and then buffered with trisodium citrate and sodium hydroxide to pH 5.8-5.9. Sulfamethazine was extracted from the aqueous mixture with methylene chloride, concentrated, dissolved in buffer, and eluted from XAD-2 resin with methanol. Sulfamethazine was reliably quantitated at 0.1 ppm by HPLC on a Zorbax ODS column with detection at 254 nm with no interference from tissues or reagents. The average recovery from the edible tissues, i.e., liver, muscle, kidney, and fat, fortified at 0.1-0.4 ppm was 85.6 +/- 3.7%.
已开发出一种高压液相色谱(HPLC)方法,用于测定猪肝、肾、肌肉和脂肪中的磺胺二甲嘧啶残留量。样品用丙酮 - 氯仿萃取,在稀盐酸存在下浓缩,然后在稀盐酸和己烷之间进行分配。酸溶液先用二氯甲烷洗涤,然后用柠檬酸钠和氢氧化钠缓冲至pH 5.8 - 5.9。磺胺二甲嘧啶用二氯甲烷从水性混合物中萃取,浓缩,溶解在缓冲液中,并用甲醇从XAD - 2树脂上洗脱。通过在Zorbax ODS柱上进行HPLC,在254 nm处检测,磺胺二甲嘧啶在0.1 ppm时可可靠定量,不受组织或试剂的干扰。在0.1 - 0.4 ppm加标的可食用组织(即肝脏、肌肉、肾脏和脂肪)中的平均回收率为85.6 +/- 3.7%。