摘要
建立了液相色谱-电喷雾串联质谱法测定鱼肉中氯霉素残留的检测方法.氘代氯霉素(d5-CAP)为内标,样品经乙酸乙酯提取,30%甲醇-正己烷去脂,固相萃取柱净化,乙腈-水(1+1)为流动相,C18色谱柱进行分离,负离子模式检测,氯霉素m/z 321/152,321/194,321/257,氘代氯霉素325.5/156.5为监控离子对,以m/z 321/152,325.5/156.5峰面积作内标法定量.方法的回收率在92.8%～108%,相对标准偏差为1.9%～9.3%,检出限低于0.01 μg·kg-1.
A sensitive method for the determination of chloramphenicol in fish by hyphenated HPLC and ESI- MS was proposed. The fish sample, after a preliminary treatment, was extracted with ethyl acetate to transfer chloramphenicol into the organic phase which after dried by blowing with nitrogen was defatted with methanol and n-hexane and purified on solid-phase extraction column （Waters Oasis HLB）. Chloramphenicol was eluated from the HLB column with methanol, and the dried eluate was separated by HPLC with Zorbax SB C18 as chromatographic column （150 mm×2.1 mm, i.d. 5μm） and with methyl cyanide-water （1＋1） solution as the mobile phase. MS detection was performed by the negative electronspray ionization and multiple reaction monitoring mode. The precursor ion of chloramphenicol with m/z of 321.0 yielded 3 main product ions with m/z of 152. 0, 194. 0 and 257. 0. Deuterium substituted chloramphenicol （ds-CAP） was used as internal standard, added to the sample before extraction with ethyl acetate The precursor ion of d5-CAP with m/z 325. 5 yielded a product ion with m/z of 156. 5. The peak areas of m/z 321.0/152.0 and 325.5/156. 5 were used in the quantitative analysis. RSD＇s of less than 9.3% and recoveries in the range from 92. 8% to 108. 0% were obtained in the test for precision and recovery. Detection limit of this method was found to be 0.01 μg · kg^-1.
出处
《理化检验（化学分册）》
CAS
CSCD
北大核心
2005年第11期799-801,共3页
Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
