检验检疫学刊
檢驗檢疫學刊
검험검역학간
INSPECTION AND QUARANTINE SCIENCE
2013年
6期
44-49
,共6页
张林田%林文%陆奕娜%林超
張林田%林文%陸奕娜%林超
장림전%림문%륙혁나%림초
UPLC-MS/MS%克伦特罗%苯乙醇胺A%莱克多巴胺%β-受体激动剂
UPLC-MS/MS%剋倫特囉%苯乙醇胺A%萊剋多巴胺%β-受體激動劑
UPLC-MS/MS%극륜특라%분을순알A%래극다파알%β-수체격동제
UPLC MS-MS%Phenylthanolamine A%Ractoppamine%Clenbuterol%β2-Agonists
研究了动物性制品中苯乙醇胺A、莱克多巴胺、克仑特罗、马步特罗残留的超高效液相色谱-串联质谱测定方法。样品经酶解、PCX固相萃取柱净化浓缩后用C18色谱柱分离,以乙酸铵与乙腈为流动相进行梯度洗脱,串联四极杆质谱检测器检测,内标法定量分析。化合物在0-10μg/kg范围内的标准曲线相关系数均≥0.999,定量检出限均为0.5μg/kg;0.5μg/kg、1.0μg/kg、5.0μg/kg 3个浓度添加水平的回收率为70.2%-119.8%,相对标准偏差为3.8%-19.1%。本方法具有简便快捷、灵敏度高、选择性强,定性准确等特点。
研究瞭動物性製品中苯乙醇胺A、萊剋多巴胺、剋崙特囉、馬步特囉殘留的超高效液相色譜-串聯質譜測定方法。樣品經酶解、PCX固相萃取柱淨化濃縮後用C18色譜柱分離,以乙痠銨與乙腈為流動相進行梯度洗脫,串聯四極桿質譜檢測器檢測,內標法定量分析。化閤物在0-10μg/kg範圍內的標準麯線相關繫數均≥0.999,定量檢齣限均為0.5μg/kg;0.5μg/kg、1.0μg/kg、5.0μg/kg 3箇濃度添加水平的迴收率為70.2%-119.8%,相對標準偏差為3.8%-19.1%。本方法具有簡便快捷、靈敏度高、選擇性彊,定性準確等特點。
연구료동물성제품중분을순알A、래극다파알、극륜특라、마보특라잔류적초고효액상색보-천련질보측정방법。양품경매해、PCX고상췌취주정화농축후용C18색보주분리,이을산안여을정위류동상진행제도세탈,천련사겁간질보검측기검측,내표법정량분석。화합물재0-10μg/kg범위내적표준곡선상관계수균≥0.999,정량검출한균위0.5μg/kg;0.5μg/kg、1.0μg/kg、5.0μg/kg 3개농도첨가수평적회수솔위70.2%-119.8%,상대표준편차위3.8%-19.1%。본방법구유간편쾌첩、령민도고、선택성강,정성준학등특점。
The method for detecting 4 kinds of β2-agonists residues such as phenylthanolamine A, ractoppamine and mabuterol, clenbuterol in animal source food was established by UPLC MS-MS. The sample was hydrolyzed byβ-glucuronidase glycosidase/aryl and the supernate was purified by PCX solid phase extraction column. Target compound could be obtained by separation through C18 chromatographic column with ammonium acetate and acetonitrile as mobile phase to gradient elute. Tandem Quadrupole Mass Spectrometry was used for final detection with internal standard in the standard curve to quantify. The quantitative detection limit was 0.5μg/kg. The recoveries of three concentration levels as 0.5μg/kg, 1.0μg/kg and 5.0μg/kg were within 70.2%-119.8%. The relative standard deviations were within 3.8%-19.1%. This method showed the characteristics of simple, fast, high sensitivity, strong selectivity, and qualitative accuracy.