分析仪器
分析儀器
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ANALYTICAL INSTRUMENTATION
2013年
6期
98-103
,共6页
徐娜%王亚立%王爱芹%任召珍%刘志敏
徐娜%王亞立%王愛芹%任召珍%劉誌敏
서나%왕아립%왕애근%임소진%류지민
液相色谱串联质谱法%大环内酯类药物%猪肉
液相色譜串聯質譜法%大環內酯類藥物%豬肉
액상색보천련질보법%대배내지류약물%저육
liquid chromatography tandem mass spectrometry (LC-MS-MS)%macrolide%pork
采用高效液相色谱-电喷雾串联质谱仪(LC -ESI-MS-MS),建立猪肉中林可霉素、竹桃霉素、替米考星、泰乐菌素、克林霉素、吉他霉素、交沙霉素等7种大环内酯类药物残留的检测方法,试验中猪肉中大环内酯类抗生素的残留用乙腈提取,以罗红霉素作为内标,提取液用正己烷去除脂肪后浓缩,再用磷酸盐溶液溶解后,经HLB固相萃取柱净化,甲醇洗脱,洗脱液浓缩定容至1mL ,供液相色谱-串联质谱法测定,内标法定量。本方法采用10μg/kg ,20μg/kg ,100μg/kg ,3个添加浓度,每个浓度6个平行样品,上述7种大环内酯类药物残留的回收率在75%~100%,相对偏差在1.51%~5.48%。
採用高效液相色譜-電噴霧串聯質譜儀(LC -ESI-MS-MS),建立豬肉中林可黴素、竹桃黴素、替米攷星、泰樂菌素、剋林黴素、吉他黴素、交沙黴素等7種大環內酯類藥物殘留的檢測方法,試驗中豬肉中大環內酯類抗生素的殘留用乙腈提取,以囉紅黴素作為內標,提取液用正己烷去除脂肪後濃縮,再用燐痠鹽溶液溶解後,經HLB固相萃取柱淨化,甲醇洗脫,洗脫液濃縮定容至1mL ,供液相色譜-串聯質譜法測定,內標法定量。本方法採用10μg/kg ,20μg/kg ,100μg/kg ,3箇添加濃度,每箇濃度6箇平行樣品,上述7種大環內酯類藥物殘留的迴收率在75%~100%,相對偏差在1.51%~5.48%。
채용고효액상색보-전분무천련질보의(LC -ESI-MS-MS),건립저육중림가매소、죽도매소、체미고성、태악균소、극림매소、길타매소、교사매소등7충대배내지류약물잔류적검측방법,시험중저육중대배내지류항생소적잔류용을정제취,이라홍매소작위내표,제취액용정기완거제지방후농축,재용린산염용액용해후,경HLB고상췌취주정화,갑순세탈,세탈액농축정용지1mL ,공액상색보-천련질보법측정,내표법정량。본방법채용10μg/kg ,20μg/kg ,100μg/kg ,3개첨가농도,매개농도6개평행양품,상술7충대배내지류약물잔류적회수솔재75%~100%,상대편차재1.51%~5.48%。
A method was established for the determination of seven kinds of macrolide drug residue in pork ,seven kinds of macrolide drug were lincomycin ,oleandomycin ,tilmicosin ,tylosin ,clindamycin , kitasamycin ,josamycin. The sample was extracted with acetonitrile. With roxithromycin as an internal standard ,extract was washed with n-hexane to remove fat and then concentrated ,phosphate solution dis-solved ,cleaned by the HLB solid phase extraction (SPE) ,methanol eluate and concentrated to volume 1mL ,for liquid chromatography-tandem mass spectrometry determination ,internal standard. This method uses 10μg/kg ,20μg/kg ,100μg/kg ,3 spiked concentration ,each concentration six parallel samples .The seven kinds of macrolide drug residues recovery is 75%-100% ,the relative deviation is 1.51%-5.48%.