食品安全质量检测学报
食品安全質量檢測學報
식품안전질량검측학보
FOOD SAFETY AND QUALITY DETECTION TECHNOLOGY
2014年
4期
1155-1165
,共11页
黄泓%夏苏捷%刘畅%王柯
黃泓%夏囌捷%劉暢%王柯
황홍%하소첩%류창%왕가
高效液相色谱-串联质谱法%β-激动剂%猪肉%猪肝
高效液相色譜-串聯質譜法%β-激動劑%豬肉%豬肝
고효액상색보-천련질보법%β-격동제%저육%저간
high performance liquid chromatography-tandem mass spectrometry%β-agonists%pork%liver
目的:建立一种用高效液相色谱-串联质谱法检测猪肉和猪肝中22种β-激动剂(特布他林、西马特罗、沙丁胺醇、非诺特罗、氯丙那林、莱克多巴胺、克仑特罗、妥布特罗、喷布特罗、福莫特罗、异丙喘宁、苯乙醇胺A、沙美特罗、马喷特罗、马布特罗、溴布特罗、苯氧丙酚胺、班布特罗、溴代克伦特罗、克仑潘特、赛布特罗和卡布特罗)的方法。方法样品粉碎后,在pH 5.2的乙酸铵缓冲液中,用β-盐酸葡萄糖醛苷酶-芳基硫酸酯酶水解,水解液经正己烷除脂后,用阳离子交换柱净化,再浓缩复溶后用高效液相色谱-串联质谱测定。采用内标法对克仑特罗、沙丁胺醇、莱克多巴胺、西马特罗、马布特罗、马喷特罗、赛布特罗和沙美特罗进行定量,其余化合物采用外标法进行定量。结果目标化合物的回收率为80%~125%,线性范围为0.5~100μg/kg,相关系数均大于0.992。方法的定量限均不大于0.5μg/kg。结论本方法灵敏、快速、简便,适合于同时定量检测猪肉和猪肝中多种β-激动剂。
目的:建立一種用高效液相色譜-串聯質譜法檢測豬肉和豬肝中22種β-激動劑(特佈他林、西馬特囉、沙丁胺醇、非諾特囉、氯丙那林、萊剋多巴胺、剋崙特囉、妥佈特囉、噴佈特囉、福莫特囉、異丙喘寧、苯乙醇胺A、沙美特囉、馬噴特囉、馬佈特囉、溴佈特囉、苯氧丙酚胺、班佈特囉、溴代剋倫特囉、剋崙潘特、賽佈特囉和卡佈特囉)的方法。方法樣品粉碎後,在pH 5.2的乙痠銨緩遲液中,用β-鹽痠葡萄糖醛苷酶-芳基硫痠酯酶水解,水解液經正己烷除脂後,用暘離子交換柱淨化,再濃縮複溶後用高效液相色譜-串聯質譜測定。採用內標法對剋崙特囉、沙丁胺醇、萊剋多巴胺、西馬特囉、馬佈特囉、馬噴特囉、賽佈特囉和沙美特囉進行定量,其餘化閤物採用外標法進行定量。結果目標化閤物的迴收率為80%~125%,線性範圍為0.5~100μg/kg,相關繫數均大于0.992。方法的定量限均不大于0.5μg/kg。結論本方法靈敏、快速、簡便,適閤于同時定量檢測豬肉和豬肝中多種β-激動劑。
목적:건립일충용고효액상색보-천련질보법검측저육화저간중22충β-격동제(특포타림、서마특라、사정알순、비낙특라、록병나림、래극다파알、극륜특라、타포특라、분포특라、복막특라、이병천저、분을순알A、사미특라、마분특라、마포특라、추포특라、분양병분알、반포특라、추대극륜특라、극륜반특、새포특라화잡포특라)적방법。방법양품분쇄후,재pH 5.2적을산안완충액중,용β-염산포도당철감매-방기류산지매수해,수해액경정기완제지후,용양리자교환주정화,재농축복용후용고효액상색보-천련질보측정。채용내표법대극륜특라、사정알순、래극다파알、서마특라、마포특라、마분특라、새포특라화사미특라진행정량,기여화합물채용외표법진행정량。결과목표화합물적회수솔위80%~125%,선성범위위0.5~100μg/kg,상관계수균대우0.992。방법적정량한균불대우0.5μg/kg。결론본방법령민、쾌속、간편,괄합우동시정량검측저육화저간중다충β-격동제。
Objective An analytical method was developed for determination of 22 β-agonists in pork and pork liver, including terbutaline, cimaterol, salbutamol, fenoterol, clorprenaline, ractopamine, clenbuterol, tulobutero, penbutolol, formoterol, metaproterenol, phenylethanolamine A, salmeterol, mapenterol, mabuterol, brombuterol, isoxsuprine, bambuterol, bromoclenbuterol, clenpenterol, cimbuterol and carbuterol by high performance liquid chromatography-tandem mass spectrometry. Methods Samples were enzymatically hydrolysed and extracted by acetic acid buffer (pH5.2). The supernatant was transferred and defatted by n-hexane, and then MCX was used as solid phase extraction cartridges to purify. The eluate was dried and reconstituted. Ractopamine, clenbuterol, salbutamol, salmeterol, mapentero, mabuterol, cimbuterol and cimaterol were determined by internal standard, others were determined by external standard. Results Average recoveries of the 22β-agonists ranged from 80%to 125%, and the calibration curves were between the concentrations of 0.5~100.0 μg/kg with the correlation coefficient r>0.992. The limit of quantitation is not more than 0.5μg/kg. Conclusion Due to its high sensitivity, accuracy and efficiency, the method is suitable for food safety control.