CAJ | 학술논문

目的：建立同时检测奶制品(牛奶、奶粉、奶酪)中9种β-受体阻断剂(β-blockers, BBS)残留的液相色谱-串联质谱方法。方法混合均匀的试样经β-葡糖醛苷酶/芳基硫酸酯酶水解,乙腈提取,硅藻土与BondElut分散固相萃取填料双重快速净化后,利用液相色谱-串联质谱法进行定性定量分析。结果9种BBs在0.1~20.0μg/L线性范围内线性关系良好(r≥0.995)；定量限(limit of quantity, LOQ,S/N≥10),均达到0.5μg/kg；3个添加水平(0.5、1.0和5.0μg/kg)下的回收率为89.5%~112.5%；相对标准偏差(relative standard deviation, RSD)为4.2%~11.5%。结论该方法快速、准确、灵敏,可用于奶制品样品中多种BBs残留的同时有效测定。
목적：건립동시검측내제품(우내、내분、내락)중9충β-수체조단제(β-blockers, BBS)잔류적액상색보-천련질보방법。방법혼합균균적시양경β-포당철감매/방기류산지매수해,을정제취,규조토여BondElut분산고상췌취전료쌍중쾌속정화후,이용액상색보-천련질보법진행정성정량분석。결과9충BBs재0.1~20.0μg/L선성범위내선성관계량호(r≥0.995)；정량한(limit of quantity, LOQ,S/N≥10),균체도0.5μg/kg；3개첨가수평(0.5、1.0화5.0μg/kg)하적회수솔위89.5%~112.5%；상대표준편차(relative standard deviation, RSD)위4.2%~11.5%。결론해방법쾌속、준학、령민,가용우내제품양품중다충BBs잔류적동시유효측정。
Objective To establish a method to simultaneously detect nineβ-blockers (BBs) such as ateenolol, pindolol, acebutolol, metoprolol, carazolol, labetalol, bisoprolol, propranolol and penbutolol in dairy products (milk, milk powder and cheese).MethodsThe samples were hydrolyzed byβ-glucuronidase/aryl sulfatase and extracted with acetonitrile, followed by continuous purification procedure of disperse solid phase extraction (d-SPE) with diatomaceous earth and BondElut cartridge. The analytes were separated by liquid chromatography and determined by liquid chromatography-tandem spectrometry under electrospray ion and multiple reaction monitor (sMRM) mode.ResultsFor the quantification, stable isotope-labelled of the analytes were used as internal standards. Over the linear range of 0.1~20.0μg/L, the correlation coefficients (r) for each BBs was no less than 0.995. The limits of quantification (limit of quantity, LOQ,S/N≥10) of all analytes were 0.5μg/kg. Recoveries from the spiked samples at three levels (0.5, 1.0 and 5.0μg/kg) ranged from 89.5% to 112.5% with the relative standard deviation from 4.2% to 11.5%. Conclusion The proposed method can be used to screen and confirm 9 BBs in a single run, which was effective in residue surveillance and detection of BBs in dairy products.