分析测试学报
分析測試學報
분석측시학보
JOURNAL OF INSTRUMENTAL ANALYSIS
2009年
7期
834-837,841
,共5页
蒋原%沈崇钰%姚义刚%丁涛%贾涛%赵厚民%徐锦忠
蔣原%瀋崇鈺%姚義剛%丁濤%賈濤%趙厚民%徐錦忠
장원%침숭옥%요의강%정도%가도%조후민%서금충
高效液相色谱-串联质谱%磺胺类药物增效剂%动物源性食品%三甲氧苄氨嘧啶%二甲氧苄氨嘧啶%奥美普林
高效液相色譜-串聯質譜%磺胺類藥物增效劑%動物源性食品%三甲氧芐氨嘧啶%二甲氧芐氨嘧啶%奧美普林
고효액상색보-천련질보%광알류약물증효제%동물원성식품%삼갑양변안밀정%이갑양변안밀정%오미보림
high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)%sulfonamides potentiator%animal origin food%trimethoprim(TMP)%diaveridine(DVD)%ormetoprim(OMP)
利用高效液相色谱-电喷雾串联质谱测定了蜂蜜、蜂王浆、鮰鱼、鳗鱼、猪肉、猪肾、猪肝、鸡肉、牛肉和牛奶中的三甲氧苄氨嘧啶、二甲氧苄氨嘧啶和奥美普林3种磺胺类药物增效剂.除蜂王浆基质直接用10%三氯乙酸溶液提取外,其余基质均用10%三氯乙酸-乙腈(体积比7 : 3)混合溶液提取,提取溶液过阳离子交换固相萃取柱进行富集和净化.采用C18色谱柱,流动相为甲醇和0.1%甲酸溶液.选择1个母离子和2个子离子进行反应监测,对3种磺胺类药物增效剂残留进行定性,选择信号最强的子离子进行定量.在2 ~100 μg/L范围内,分析物的线性相关系数r>0.992.通过实际样品添加回收实验,所有基质定量下限为5.0 μg/kg,3个添加水平的回收率为63% ~89%,相对标准偏差为3.2% ~6.9%.
利用高效液相色譜-電噴霧串聯質譜測定瞭蜂蜜、蜂王漿、鮰魚、鰻魚、豬肉、豬腎、豬肝、鷄肉、牛肉和牛奶中的三甲氧芐氨嘧啶、二甲氧芐氨嘧啶和奧美普林3種磺胺類藥物增效劑.除蜂王漿基質直接用10%三氯乙痠溶液提取外,其餘基質均用10%三氯乙痠-乙腈(體積比7 : 3)混閤溶液提取,提取溶液過暘離子交換固相萃取柱進行富集和淨化.採用C18色譜柱,流動相為甲醇和0.1%甲痠溶液.選擇1箇母離子和2箇子離子進行反應鑑測,對3種磺胺類藥物增效劑殘留進行定性,選擇信號最彊的子離子進行定量.在2 ~100 μg/L範圍內,分析物的線性相關繫數r>0.992.通過實際樣品添加迴收實驗,所有基質定量下限為5.0 μg/kg,3箇添加水平的迴收率為63% ~89%,相對標準偏差為3.2% ~6.9%.
이용고효액상색보-전분무천련질보측정료봉밀、봉왕장、회어、만어、저육、저신、저간、계육、우육화우내중적삼갑양변안밀정、이갑양변안밀정화오미보림3충광알류약물증효제.제봉왕장기질직접용10%삼록을산용액제취외,기여기질균용10%삼록을산-을정(체적비7 : 3)혼합용액제취,제취용액과양리자교환고상췌취주진행부집화정화.채용C18색보주,류동상위갑순화0.1%갑산용액.선택1개모리자화2개자리자진행반응감측,대3충광알류약물증효제잔류진행정성,선택신호최강적자리자진행정량.재2 ~100 μg/L범위내,분석물적선성상관계수r>0.992.통과실제양품첨가회수실험,소유기질정량하한위5.0 μg/kg,3개첨가수평적회수솔위63% ~89%,상대표준편차위3.2% ~6.9%.
A high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)method was developed for determination of three potentiators,e.g.trimethoprim(TMP),diaveridine(DVD) and ormetoprim(OMP) in honey,royal jelly,catfish,eel,pork,porcine kidney,porcine liver,chicken,beef and milk samples.Except that the royal jelly samples was directly extracted by 10%trichloroacetic acid solution,other matrices samples were extracted by 10%trichloroacetic acid-acetonitrile(7 : 3,by volume).The extracts were concentrated and purified by cation-exchange solid phase extraction cartridge.The separation of analytes was performed on C18 analytical chromatographic column with a gradient elution using methanol(A) and 0.1%formic acid(B) solution as mobile phase.The analysis of three potentiators were performed under selective reaction monitoring(SRM) mode by selecting one parent ion and two daughter ions as qualitative ions,and the most abundant daughter ion as a quantitative ion.The calibration curves of three potentiators were linear in the concentration range of 2-100 μg/L with correlation coefficients more than 0.992.The quantitative limits of the method were 5 μg/kg for all matrices,and the spiked recoveries were in the range of 63%-89%with RSDs of 3.2%-6.9%.