福建水产
福建水產
복건수산
JOURNAL OF FUJIAN FISHERIES
2012年
5期
375-381
,共7页
磺胺类药物%混合型阳离子交换固相萃取柱%高效液相色谱%鳗鲡
磺胺類藥物%混閤型暘離子交換固相萃取柱%高效液相色譜%鰻鱺
광알류약물%혼합형양리자교환고상췌취주%고효액상색보%만려
sulfonamides%mixed mode cation exchange solid phase extraction column%high performance liquid chromatography%eel
针对鳗鲡基质油脂较多的特点,建立了一种同时测定鳗鲡体中13种磺胺类药物残留的固相萃取-高效液相色谱方法。样品用乙酸乙酯提取,浓缩后用盐酸溶解,正己烷除脂,经混合型阳离子交换固相萃取柱净化后,用高效液相色谱分离,DAD检测器检测,外标法定量。13种磺胺类药物在0.01～2.0μg/mL范围内线性关系良好,相关系数R2≥0.9999,平均加标回收率为71.7%～89.8%,相对标准偏差为0.80%～7.82%。方法检出限为3.05～5.24μg/kg,定量限为10.1～17.5μg/kg。
針對鰻鱺基質油脂較多的特點,建立瞭一種同時測定鰻鱺體中13種磺胺類藥物殘留的固相萃取-高效液相色譜方法。樣品用乙痠乙酯提取,濃縮後用鹽痠溶解,正己烷除脂,經混閤型暘離子交換固相萃取柱淨化後,用高效液相色譜分離,DAD檢測器檢測,外標法定量。13種磺胺類藥物在0.01～2.0μg/mL範圍內線性關繫良好,相關繫數R2≥0.9999,平均加標迴收率為71.7%～89.8%,相對標準偏差為0.80%～7.82%。方法檢齣限為3.05～5.24μg/kg,定量限為10.1～17.5μg/kg。
침대만려기질유지교다적특점,건립료일충동시측정만려체중13충광알류약물잔류적고상췌취-고효액상색보방법。양품용을산을지제취,농축후용염산용해,정기완제지,경혼합형양리자교환고상췌취주정화후,용고효액상색보분리,DAD검측기검측,외표법정량。13충광알류약물재0.01～2.0μg/mL범위내선성관계량호,상관계수R2≥0.9999,평균가표회수솔위71.7%～89.8%,상대표준편차위0.80%～7.82%。방법검출한위3.05～5.24μg/kg,정량한위10.1～17.5μg/kg。
A solid phase extraction and high performance liquid chromatographic method has been developed for the simultaneous determination of thirteen sulfonamides residues in eel products.The samples were extracted with ethyl acetate,concentrated and dissolved with hydrochloric acid,then cleaned up by n-hexane liquid-liquid extraction and solid phase extraction.The residues were determined by high performance liquid chromatography with diode array detector and quantified by external standard method.The linear ranges were 0.01~2.0 mg/L with the correlation coefficient over 0.9999.The average recoveries in spiked samples were found to be in the range of 71.7%~89.8% with relative standard deviation of 0.80%~7.82%.The limits of detection were found to be 3.05~5.24 μg/kg and the limits of quantification 10.1~17.5 μg/kg.
