干旱区生态环境知识资源中心(Arid): 超高效液相色谱-电喷雾串联质谱法对饲料中匹莫林的测定

Arid

	超高效液相色谱-电喷雾串联质谱法对饲料中匹莫林的测定
其他题名	Determination of Pemoline in Feeds Using Ultra-performance Liquid Chromatography-Electrospray Tandem Mass Spectrometry
	班付国; 方忠意; 刘素梅; 宋志超; 贾振民; 吴宁鹏
ISSN	1004-4957
出版年	2009
卷号	28 期号:6 页码:705-708
中文摘要	建立了超高效液相色谱-串联质谱测定饲料中匹莫林的方法.饲料样品经甲醇-乙腈溶液提取,取部分上清液氮气吹干,用甲醇和水分步溶解后用正己烷除脂,Waters Oasis HLB固相萃取小柱净化,然后用Waters Acquity UPLC BEH C_18色谱柱(2.1 mm*50 mm i.d.,1.7 mum)分离,以甲醇和0.1%甲酸-水溶液为流动相进行梯度洗脱,外标法定量.对前处理及液相色谱和质谱条件进行优化.结果表明,匹莫林质量浓度在1 ～500 mug/L范围内线性良好,相关系数大于0.999;在5.0 ～200 mug/kg的添加水平下,匹莫林的平均加标回收率为77% ～86%;相对标准偏差为4.4% ～7.9%;方法的检出限低至2.0 mug/kg,定量下限低至5.0 mug/kg.该方法灵敏度高、稳定性好,可满足饲料中匹莫林残留的检测与确证的要求.
英文摘要	An ultra-performance liquid chromatographic method with tandem mass spectrometric determination was developed for determination of pemoline in feeds. The sample was extracted by meth-anol - acetonitrile solution. The extract was evaporated to dryness under nitrogen, and redissolved by methanol and water, sequencely. The mixture was degreased by ethyl acetate and cleaned up on a Waters Oasis HLB solid phase extraction column. The separation of compounds was carried on a BEH C_18 column(2. 1 mm *50 mm i. d. , 1. 7 mum) by a gradient elution using methanol( A) -water( added 0. 1 % formic acid) (B) as mobile phase with a flow rate of 0. 3 mL/min. The analyte was detected by tandem quadrupole mass spectrometry under multiple reaction monitoring ( MRM) mode with positive electrospray ionization(ESI). The method was quantified by external standard method. The experimental conditions were optimized. Under the optimal conditions, the calibration curve showed a good linearity over the concentration of pemoline in the range of 1 - 500 mug/L with a correlation coefficient more than 0. 999. The detection limit (LOD) and the quantitative limit (LOQ) of pemoline were 2. 0 mug/kg and 5.0 mug/kg, respectively. The average recoveries from spiked feeds samples at four concentration levels of 5.0, 10, 50 and 200 mug/kg ranged from 77% to 86% with relative standard deviations of 4.4% -7.9%. The method showed a good repeatability and high sensitivity, and was suitable for the determination and confirmation of pemoline in feeds.
中文关键词	匹莫林 ; 超高效液相色谱-串联质谱 ; 饲料
英文关键词	pemoline ultra-performance liquid chromatography - tandem mass spectrometry feed
语种	中文
国家	中国
收录类别	CSCD
WOS类目	CHEMISTRY ANALYTICAL ; ENGINEERING CHEMICAL
WOS研究方向	Chemistry ; Engineering
CSCD记录号	CSCD:3516843
资源类型	期刊论文
条目标识符	http://119.78.100.177/qdio/handle/2XILL650/223481
作者单位	农业部畜禽产品质量安全检验测试中心, 郑州, 河南 450008, 中国
推荐引用方式 GB/T 7714	班付国,方忠意,刘素梅,等. 超高效液相色谱-电喷雾串联质谱法对饲料中匹莫林的测定[J],2009,28(6):705-708.
APA	班付国,方忠意,刘素梅,宋志超,贾振民,&吴宁鹏.(2009).超高效液相色谱-电喷雾串联质谱法对饲料中匹莫林的测定.,28(6),705-708.
MLA	班付国,et al."超高效液相色谱-电喷雾串联质谱法对饲料中匹莫林的测定".28.6(2009):705-708.