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
2015年
1期
303-309
,共7页
张燕%徐幸%郭启新%舒平%赵用%杨朝义%赵燕娜
張燕%徐倖%郭啟新%舒平%趙用%楊朝義%趙燕娜
장연%서행%곽계신%서평%조용%양조의%조연나
磺胺吡啶%磺胺噻唑%磺胺甲基异恶唑%高效液相色谱-串联质谱法%牛奶%不确定度
磺胺吡啶%磺胺噻唑%磺胺甲基異噁唑%高效液相色譜-串聯質譜法%牛奶%不確定度
광알필정%광알새서%광알갑기이악서%고효액상색보-천련질보법%우내%불학정도
sulfapyridin%sulfathiazole%sulfamethoxazole%liquid chromatography-tandem mass spectrometry%milk%uncertainty
目的:采用高效液相色谱-串联质谱法对牛奶中磺胺吡啶、磺胺噻唑和磺胺甲基异恶唑残留的不确定度进行评估。方法建立测定牛奶中磺胺吡啶、磺胺噻唑和磺胺甲基异恶唑含量不确定度的数学模型,确定不确定度来源并对其评定。结果当牛奶中磺胺吡啶含量为5.09μg/kg 时,其扩展不确定度为0.62μg/kg (k=2);当牛奶中磺胺噻唑含量为8.62μg/kg 时,其扩展不确定度为0.71μg/kg (k=2);当牛奶中磺胺甲基异恶唑含量为10.15μg/kg 时,其扩展不确定度为0.81μg/kg(k=2)。其中,测量重复性和标准曲线对不确定度的影响最大。结论影响检测结果不确定度的主要因素为样品测量的重复性、标准曲线拟合和样品的前处理过程。
目的:採用高效液相色譜-串聯質譜法對牛奶中磺胺吡啶、磺胺噻唑和磺胺甲基異噁唑殘留的不確定度進行評估。方法建立測定牛奶中磺胺吡啶、磺胺噻唑和磺胺甲基異噁唑含量不確定度的數學模型,確定不確定度來源併對其評定。結果噹牛奶中磺胺吡啶含量為5.09μg/kg 時,其擴展不確定度為0.62μg/kg (k=2);噹牛奶中磺胺噻唑含量為8.62μg/kg 時,其擴展不確定度為0.71μg/kg (k=2);噹牛奶中磺胺甲基異噁唑含量為10.15μg/kg 時,其擴展不確定度為0.81μg/kg(k=2)。其中,測量重複性和標準麯線對不確定度的影響最大。結論影響檢測結果不確定度的主要因素為樣品測量的重複性、標準麯線擬閤和樣品的前處理過程。
목적:채용고효액상색보-천련질보법대우내중광알필정、광알새서화광알갑기이악서잔류적불학정도진행평고。방법건립측정우내중광알필정、광알새서화광알갑기이악서함량불학정도적수학모형,학정불학정도래원병대기평정。결과당우내중광알필정함량위5.09μg/kg 시,기확전불학정도위0.62μg/kg (k=2);당우내중광알새서함량위8.62μg/kg 시,기확전불학정도위0.71μg/kg (k=2);당우내중광알갑기이악서함량위10.15μg/kg 시,기확전불학정도위0.81μg/kg(k=2)。기중,측량중복성화표준곡선대불학정도적영향최대。결론영향검측결과불학정도적주요인소위양품측량적중복성、표준곡선의합화양품적전처리과정。
Objective To establish a mathematical model of uncertainty evaluation of sulfapyridine, sulfathiazole and sulfamethoxazole in milk by high performance liquid chromatography-tandem mass spectrometry method. Methods To establish a mathematical model for determination of sulfapyridine, sulfathiazole and sulfamethoxazole uncertainty in milk. The sources of uncertainty of the whole determination procedure were analyzed and the combined uncertainty was finally obtained. Results The expanded uncertainty of 5.09 μg/kg (k=2) with 0.62 μg/kg of the content of sulfapyridin was derived. The expanded uncertainty of 8.62 μg/kg (k=2) with 0.71 μg/kg of the content of sulfathiazole was derived. The expanded uncertainty of 10.15 μg/kg (k=2) with 0.81 μg/kg of the content of sulfamethoxazole was derived. The major sources of uncertainty of measurement include the repeatability of detection and the curve fitting. Conclusion The major uncertainty sources were standard curve fitting;measurement repeatability and sample pretreatment.