干旱区生态环境知识资源中心(Arid): 猪可食性组织中氟尼辛残留量的UPLC-MS/MS检测方法的建立

Arid

	猪可食性组织中氟尼辛残留量的UPLC-MS/MS检测方法的建立
其他题名	Development of an ultra-performance liquid chromatography-tandem mass spectrometry method for the determination of flunixin in edible swine tissues
	罗小清; 张珍瑞; 郭凡溪; 郭洋洋; 吴峰; 余祖功
来源期刊	南京农业大学学报
ISSN	1000-2030
出版年	2017
卷号	40 期号:6 页码:1105-1110
中文摘要	[目的]建立一种可靠、快速、灵敏的超高效液相色谱-串联质谱法(UPLC-MS/MS)用于猪可食性组织中氟尼辛残留量的检测。[方法]猪可食性组织(肌肉、皮脂、肝脏、肾脏)经绞碎、均质后,用乙酸乙酯-乙腈(体积比1∶1)提取,MCX固相萃取柱净化,Acquity UPLC BEH C_(18)色谱柱梯度洗脱,在电喷雾正离子(ESI~+)下选用多反应监测(MRM)模式进行待测物的分析,外标法定量。[结果]该方法的检测限(LOD)与定量限(LOQ)分别为0.5 mug·kg~(-1)和1.0 mug·kg~(-1);待测物氟尼辛含量在0.5~500 mug·kg~(-1)范围内,峰面积与药含量呈良好的线性关系(R~2>0.999);氟尼辛在猪肌肉、皮脂、肝脏、肾脏组织中的添加回收率为74.8%~90.3%,批内精密度及批间精密度均不大于16.5%。[结论]建立了猪超高效液相色谱-串联质谱检测方法,适用于猪可食性组织中氟尼辛残留量的测定。
英文摘要	[Objectives]To establish a reliable,rapid and sensitive method for determination of flunixin residues in swine tissues(muscle,skin+fat,liver,kidney),ultra-performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)was developed and optimized. [Methods]The samples were extracted with acetonitrile and ethyl acetate(volume ratio 1∶1),and then purified via an Oasis MCX solid-phase extraction cartridge. Chromatographic separation was performed on an Acquity UPLC BEH C_(18) column. The analysis was carried out on UPLC-ESI-MS/MS working with multiple reaction monitoring mode. External standard was used for quantitation of target drug. [Results]The analyte has a good linearity at the range of 0.5-500 mug·kg~(-1),with related coefficient of R~2>0.999. Recoveries of spiked samples ranged from 74.8% to 90.3% with relative standard deviation(RSD)less than 16.5%. The limits of detection(LOD)and quantification(LOQ)were 0.5 and 1.0 mug·kg~(-1),respectively. [Conclusions]The results show that the pretreatment and purification process established by this study are easy to operate. The method has good stability,reproducibility,sensitivity,and great accuracy.
中文关键词	氟尼辛 ; 猪可食性组织 ; 残留
英文关键词	UPLC-MS/MS flunixin edible swine tissues UPLC-MS/MS residues
语种	中文
国家	中国
收录类别	CSCD
WOS类目	AGRICULTURE MULTIDISCIPLINARY
WOS研究方向	Agriculture
CSCD记录号	CSCD:6115730
资源类型	期刊论文
条目标识符	http://119.78.100.177/qdio/handle/2XILL650/236286
作者单位	南京农业大学动物医学院, 南京, 江苏 210095, 中国
推荐引用方式 GB/T 7714	罗小清,张珍瑞,郭凡溪,等. 猪可食性组织中氟尼辛残留量的UPLC-MS/MS检测方法的建立[J],2017,40(6):1105-1110.
APA	罗小清,张珍瑞,郭凡溪,郭洋洋,吴峰,&余祖功.(2017).猪可食性组织中氟尼辛残留量的UPLC-MS/MS检测方法的建立.南京农业大学学报,40(6),1105-1110.
MLA	罗小清,et al."猪可食性组织中氟尼辛残留量的UPLC-MS/MS检测方法的建立".南京农业大学学报 40.6(2017):1105-1110.