干旱区生态环境知识资源中心(Arid): 禽蛋中头孢噻肟残留的高效液相色谱-串联质谱法测定

Arid

	禽蛋中头孢噻肟残留的高效液相色谱-串联质谱法测定
其他题名	Determination of Cefotaxime Residue in Poultry Egg by High Performance Liquid Chromatography - Tandem Ma s Spectrometry
	罗辉泰; 黄晓兰; 吴惠勤; 朱志鑫; 黄芳; 林晓珊
来源期刊	分析测试学报
ISSN	1004-4957
出版年	2010
卷号	29 期号:8 页码:772-776
中文摘要	建立了高效液相色谱-串联质谱(LC-MS/MS)测定禽蛋中头孢噻肟药物残留的方法. 禽蛋样品中的头孢噻肟用纯水提取,乙腈沉淀蛋白, Oasis HLB(500 mg, 6 mL)固相萃取柱净化, 8 mL甲醇洗脱. 采用 Zorbax XDB-C_(18)(2.1 mm*50 mm, 3.5mum)色谱柱,以0.2%甲酸水-乙腈为流动相, 0.3 mL/min梯度洗脱,经高效液相色谱分离后,采用电喷雾质谱正离子模式电离,多反应选择离子检测(MRM)模式测定. 检测离子对为m/z456.1/396.1、m/z456.1/324.1,其中m/z456.1/396.1为定量离子对. 在1.35~135mug/L范围内标准曲线的线性关系良好,相关系数为0.999 3;在1.0、50.0、100mug/kg3个添加水平的平均加标回收率为87%~99%,相对标准偏差为1.9%~3.9%;方法检出限为0.3mug/kg,定量下限为1.0mug/kg. 该方法简便、灵敏、准确、可靠,适用于禽蛋中头孢噻肟药物残留的分析
英文摘要	A confirmative method to determine cefotaxime residue in poultry egg by high performance liquid chromatography - tandem mass spectrometry(HPLC - MS/MS) under multiple reaction monitoring(MRM) mode was developed. The cefotaxime in sample was extracted with water. Sample preparation involved the protein precipitation with acetonitrile and the llean-up on an Oasis HLB(500 mg, 6 mL) solid phase extraction(SPE) cartridge. The analyte was eluted from the SPE cartridge with 8 mL methanol. The separation of cefotaxime was performed on a Zorbax XDB-C_(18) (2. 1 mm x 50 mm, 3. 5 mum) column using a mobile phase of 0. 2% formic acid (A) - acetonitrile (B) by gradient elution with a flow rate of 0. 3 mL/min. The detection of cefotaxime was carried out by electrospray ionization mass spectrometry under positive mode. The MRM monitored ions, m/z 456. 1/396. 1 and m/z 456. 1/324. 1, were selected as qualitative ions, and m/z 456. 1 396. 1 was selected as quantitative ion. The calibration curve showed a good linearity in the range of 1. 35 - 135 mug/L with a correlation coefficient of 0. 999 3. The average spiked recoveries of cefotaxime at three concentration levels of 1.0, 50. 0, 100 mug/kg were between 87% and 99%, and the relative standard deviations (RSDs, n =6) ranged from 1. 9% to 3. 9%. The limit of detection(LOD, S/N≥3) and limit of quantification(LOQ, S/N≥10) were 0. 3 mug/kg and 1. 0 mug/kg, respecti ely. The results demonstrated that the method was simple, sensitive, accurate and reliable, and was suitable for the determination on cefotaxime residue in poultry egg
中文关键词	头孢噻肟 ; 高效液相色谱 ; 串联质谱 ; 禽蛋 ; 残留
英文关键词	cefotaxime high performance liquid chromatography (HPLC) tandem mass spectrometry(MS/MS) poultry egg residue
语种	中文
国家	中国
收录类别	CSCD
WOS类目	CHEMISTRY ANALYTICAL ; AGRICULTURE MULTIDISCIPLINARY
WOS研究方向	Chemistry ; Agriculture
CSCD记录号	CSCD:3969933
资源类型	期刊论文
条目标识符	http://119.78.100.177/qdio/handle/2XILL650/224913
作者单位	中国广州分析测试中心, 广州, 广东 510070, 中国
推荐引用方式 GB/T 7714	罗辉泰,黄晓兰,吴惠勤,等. 禽蛋中头孢噻肟残留的高效液相色谱-串联质谱法测定[J],2010,29(8):772-776.
APA	罗辉泰,黄晓兰,吴惠勤,朱志鑫,黄芳,&林晓珊.(2010).禽蛋中头孢噻肟残留的高效液相色谱-串联质谱法测定.分析测试学报,29(8),772-776.
MLA	罗辉泰,et al."禽蛋中头孢噻肟残留的高效液相色谱-串联质谱法测定".分析测试学报 29.8(2010):772-776.