CAJ | 학술논문

目的建立直接提取-超高压液相色谱-电喷雾串联质谱法(UPLC-ESIMS/MS)同时测定原料奶及奶粉中土霉素、四环素、金霉素、强力霉素4种四环素类药物的分析方法.方法原料奶及奶粉样品经少量高氯酸沉淀蛋白、低温冷冻除脂后,用 C18色谱柱分离,以0.1%甲酸水和乙腈为流动相进行梯度洗脱,电喷雾串联质谱正离子模式扫描,多反应监测模式(MRM)检测,外标法定量.结果4种四环素族药物在1~1000 ng/mL 浓度范围内线性关系良好,相关系数 r 均在0.993以上.本方法的定量限为(S/N≥10)为原料奶5μg/kg,奶粉25μg/kg,在10、50、100μg/kg 三个加标水平下,加标回收率为73.4%~99.4%,相对标准偏差为0.8%~14.3%(n≥6).结论该方法简便快速、灵敏可靠、经济有效,适用于原料奶及奶粉中土霉素、四环素、金霉素和强力霉素4种四环素族药物残留的测定.
목적건립직접제취-초고압액상색보-전분무천련질보법(UPLC-ESIMS/MS)동시측정원료내급내분중토매소、사배소、금매소、강력매소4충사배소류약물적분석방법.방법원료내급내분양품경소량고록산침정단백、저온냉동제지후,용 C18색보주분리,이0.1%갑산수화을정위류동상진행제도세탈,전분무천련질보정리자모식소묘,다반응감측모식(MRM)검측,외표법정량.결과4충사배소족약물재1~1000 ng/mL 농도범위내선성관계량호,상관계수 r 균재0.993이상.본방법적정량한위(S/N≥10)위원료내5μg/kg,내분25μg/kg,재10、50、100μg/kg 삼개가표수평하,가표회수솔위73.4%~99.4%,상대표준편차위0.8%~14.3%(n≥6).결론해방법간편쾌속、령민가고、경제유효,괄용우원료내급내분중토매소、사배소、금매소화강력매소4충사배소족약물잔류적측정.
@@@@Objective A method for the simultaneous determination of oxytetracycline, tetracycline, chlortetracycline, and doxycycline residues in milk and dairy products was developed using direct extraction and ultra pressure liquid chromatography-electrospray tandem mass spectrometry (UPLC-ESI-MS/MS). Me-thods Samples were extracted with little perchloric acid to precipitate protein and remove Frozen grease, se-parated by C18 column with gradient elution using acetonitrile and water (containing 0.1% formic acid) and analyzed by UPLC-ESI-MS/MS under the positive mode using multiple reaction monitoring (MRM). The sam-ples were quantified with external standard method. Results The method showed a good linearity over the range of 1~1000 ng/mL for 4 compounds of tetracycline antibiotics residue with r≥0.993. The detection limit (S/N≥10) of milk was 5 μg/kg , and that of dairy products was 25 μg/kg. The recoveries were 73.4%~99.4% at the spiked level of 10, 50 μg/kg, and 100 μg/kg with relative standard deviation of 0.8%~14.3%(n≥6). Con-clusion This method is simple, accurate and reproducible, and it is suitable for the rapid analysis of tetracy-cline antibiotics in milk and dairy products.