CAJ | 학술논문

目的：建立检测禽类组织(肌肉、脂肪、肝脏、肾脏)中黄霉素A残留的超快速液相色谱-四极杆/线性离子阱质谱方法。方法混合均匀的试样经10%氨化甲醇提取,乙腈沉降蛋白净化后,以0.3%甲酸-5%乙腈-水溶液和0.3%甲酸―5%水-乙腈为流动相,使用Agilent Poroshell 120 SB-C18(100 mm×2.1 mm,2.7μm)色谱柱超快速液相色谱分离,优化多反应检测(selected multiple reaction monitorin g, sMRM)模式检测,外标法定量。结果黄霉素A在20~200μg/L线性范围内线性关系良好(r≥0.995)；黄霉素A定量限(limit of quantity, LOQ, S/N≥10)为10μg/kg；3个添加水平(10、20和100μg/kg)下的回收率为66.5%~89.4%；相对标准偏差(relative standard deviation, RSD)为4.7%~10.2%。结论该方法快速、准确、灵敏,可有效用于禽类组织中黄霉素A残留的测定。
목적：건립검측금류조직(기육、지방、간장、신장)중황매소A잔류적초쾌속액상색보-사겁간/선성리자정질보방법。방법혼합균균적시양경10%안화갑순제취,을정침강단백정화후,이0.3%갑산-5%을정-수용액화0.3%갑산―5%수-을정위류동상,사용Agilent Poroshell 120 SB-C18(100 mm×2.1 mm,2.7μm)색보주초쾌속액상색보분리,우화다반응검측(selected multiple reaction monitorin g, sMRM)모식검측,외표법정량。결과황매소A재20~200μg/L선성범위내선성관계량호(r≥0.995)；황매소A정량한(limit of quantity, LOQ, S/N≥10)위10μg/kg；3개첨가수평(10、20화100μg/kg)하적회수솔위66.5%~89.4%；상대표준편차(relative standard deviation, RSD)위4.7%~10.2%。결론해방법쾌속、준학、령민,가유효용우금류조직중황매소A잔류적측정。
Objective To establish a highly sensitive method to confirm moenomycin A residues in poultry tissues (muscle, fat, liver and kidney) by liquid chromatography-tandem mass spectrometry (LC-MS/MS).Methods The poultry tissues were extracted with 10% ammoniation of methanol, and purified by acetonitrile. The chromatography separation was conducted on an Agilent Poroshell 120 SB-C18 column (100 mm×2.1 mm, 2.7μm) with a mobile phase of 0.3% formic acid-5%acetonitrile–water (v:v:v) and 0.3% formic acid-5% water-acetonitrile (v:v:v) with gradient elution. The analytes were separated by LC and determined by LC-MS/MS and multiple reaction monitor (selected multiple reaction monitoring, sMRM) mode. External standard was used for the quantification.Results Moenomycin A showed a good linearity with the correlation coefficients (r) no less than 0.995 in the range of 20~200μg/L, with the limits of quantification (limit of quantity, LOQ,S/N≥10) of 10μg/kg for all analytes. The developed method gave average recoveries of 66.5%~89.4% for drugs spiked at 10~100μg/kg, with the relative standard deviation of 4.7%~10.2%.Conclusion The proposed method could be used to screen and confirm moenomycin A in a single run, which made it effective in residue surveillance and detection of moenomycin A in poultry tissues.