干旱区生态环境知识资源中心(Arid): 液相色谱-电喷雾串联质谱法测定鱼肉中氯霉素含量

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	液相色谱-电喷雾串联质谱法测定鱼肉中氯霉素含量
其他题名	HPLC-ESI-MS DETERMINATION OF CHLORAMPHENICOL IN FISH
	瞿进文; 吴洁珊; 蔡勤仁; 黄新民; 古学群; 陈伟生
来源期刊	理化检验. B, 化学分册
ISSN	1001-4020
出版年	2005
卷号	41 期号:11 页码:799-801
中文摘要	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 mug·kg-1.
英文摘要	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 Ci8 as chromatographic column (150 mmX2. 1 mm, i. d. 5 ^m) 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 mlz of 152. 0, 194. 0 and 257. 0. Deuterium substituted chloramphenicol (dsCAP) was used as internal standard, added to the sample before extraction with ethyl acetate. The precursor ion of do-CAP with mlz 325. 5 yielded a product ion with mlz of 156. 5. The peak areas of mlz 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 fxg ? kg"1.
中文关键词	液相色谱-串联质谱 ; 鱼 ; 氯霉素
英文关键词	HPLC-ESI-MS Fish Chloramphenicol
语种	中文
国家	中国
收录类别	CSCD
WOS类目	CHEMISTRY ANALYTICAL
WOS研究方向	Chemistry
CSCD记录号	CSCD:2129071
资源类型	期刊论文
条目标识符	http://119.78.100.177/qdio/handle/2XILL650/206421
作者单位	珠海出入境检验检疫局, 珠海, 广东 519020, 中国
推荐引用方式 GB/T 7714	瞿进文,吴洁珊,蔡勤仁,等. 液相色谱-电喷雾串联质谱法测定鱼肉中氯霉素含量[J],2005,41(11):799-801.
APA	瞿进文,吴洁珊,蔡勤仁,黄新民,古学群,&陈伟生.(2005).液相色谱-电喷雾串联质谱法测定鱼肉中氯霉素含量.理化检验. B, 化学分册,41(11),799-801.
MLA	瞿进文,et al."液相色谱-电喷雾串联质谱法测定鱼肉中氯霉素含量".理化检验. B, 化学分册 41.11(2005):799-801.