CAJ | 학술논문

目的：建立同时测定乳制品中氯霉素、甲砜霉素和氟甲砜霉素的液质联用方法。方法样品经乙腈提取,饱和乙腈正己烷脱脂,以甲醇水作为流动相,通过高效液相色谱,采用负离子模式多反应监测,氯霉素用同位素内标定量,甲砜霉素、氟甲砜霉素用外标法定量。结果本方法线性范围：0.25~20.0μg/L,相关系数＞0.999,检出限0.01μg/kg,定量限0.1μg/kg,三种物质添加水平分别为0.5、2.5、5.0μg/kg,加标回收率分别为氯霉素82.2~103%,甲砜霉素81.8~108%,氟甲砜霉素67.6~104%, RSD<10%。结论该方法具有简单快速、灵敏度高、准确性强等特点,适用于测定乳及乳制品中氯霉素、甲砜霉素和氟甲砜霉素的含量。
목적：건립동시측정유제품중록매소、갑풍매소화불갑풍매소적액질련용방법。방법양품경을정제취,포화을정정기완탈지,이갑순수작위류동상,통과고효액상색보,채용부리자모식다반응감측,록매소용동위소내표정량,갑풍매소、불갑풍매소용외표법정량。결과본방법선성범위：0.25~20.0μg/L,상관계수＞0.999,검출한0.01μg/kg,정량한0.1μg/kg,삼충물질첨가수평분별위0.5、2.5、5.0μg/kg,가표회수솔분별위록매소82.2~103%,갑풍매소81.8~108%,불갑풍매소67.6~104%, RSD<10%。결론해방법구유간단쾌속、령민도고、준학성강등특점,괄용우측정유급유제품중록매소、갑풍매소화불갑풍매소적함량。
ABSTRACT:ObjectiveA high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) analysis method was established for simultaneous determination of chloramphenicol, thiamphenicol and florfenicol in milk and dairy products.Methods The sample was extracted with acetonitrile and degreased with saturated acetonitrile n-hexane. Mobile phase was methanol and water. The identification and quantification ofchloramphenicols residues were carried out by MS/MS in negative electrospray ionization (ESI) and multiple reaction monitoring (MRM) mode. Using isotope internal standard quantitation of chloramphenicol, thiamphenicol and florfenicol by external standard method for quantitative. Results The calibration curve showed a good linearity in the range of 0.25~20.0μg/L with the correlation coefficientr2>0.999. The detection limit was 0.01μg/kg. The quantification (LOQ) limit was 0.1μg/kg. The average recoveries of chloramphenicol, thiamphenicol and florfenicol spiked at 0.5, 2.5μg/kg and 5.0μg/kg levels in different matrix were 82.2%~103%, 81.8%~108% and 67.6%~104%. The relative standard deviations were less than 10%. Conclusion This method is simple, effective and sensitive, and it is suitable for the determination of chloramphenicol, thiamphenicol and florfenicol in milk and dairy products.