干旱区生态环境知识资源中心(Arid): 固相萃取-超高效液相色谱-串联质谱法测定饲料中沃尼妙林和泰妙菌素

Arid

	固相萃取-超高效液相色谱-串联质谱法测定饲料中沃尼妙林和泰妙菌素
其他题名	Determination of Valnemulin and Tiamulin in Feed by Solid Phase Extraction-Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry
	王凤芹; 杨媛媛; 陈楚昊; 胡喻涵; 路则庆; 汪以真
来源期刊	动物营养学报
ISSN	1006-267X
出版年	2018
卷号	30 期号:6 页码:2394-2401
中文摘要	本试验旨在建立一种高效快速测定饲料中沃尼妙林和泰妙菌素的固相萃取-超高效液相色谱-串联质谱方法。用甲醇提取饲料中的沃尼妙林和泰妙菌素,经过Oasis MCX固相萃取柱净化后,由C18色谱柱分离,流动相为水(含0.1%甲酸)-乙腈(含0.1%甲酸),梯度洗脱,以电喷雾离子源(ESI)正离子扫描方式,在多反应监测(MRM)模式下进行测定,外标法定量。结果表明:本试验建立的固相萃取-超高效液相色谱-串联质谱法对饲料中沃尼妙林和泰妙菌素的检测限分别为25.0和5.0 ng/g。沃尼妙林和泰妙菌素浓度在0.01~ 5.00 mug/mL范围内线性关系良好,相关系数(R~2)均大于0.99。在3个添加水平(2.5、25.0、125.0 mg/kg)下,沃尼妙林的回收率为85.17%~ 94.55%,相对标准偏差(RSD)为2.56%~ 7.65%,泰妙菌素的回收率为84.69%~ 99.36%,RSD为1.57%~ 4.95%。结果表明,本试验建立的固相萃取-超高效液相色谱-串联质谱法操作简单、准确度高,可应用于饲料中沃尼妙林和泰妙菌素的快速定量测定。
英文摘要	This experiment was conducted to develop a fast and effective method for the determination of valnemulin and tiamulin in feed by solid phase extraction-ultra performance liquid chromatography-tandem mass spectrometry (SPE-UPLC-MS/MS). After the feed sample was extracted by methanol and cleaned-up on an Oasis MCX solid phase extraction (SPE) column, the valnemulin and tiamulin were separated by a C18 chromatographic column with gradient elution using 0.1% formic acid in water and 0.1% formic acid in acetonitrile as mobile phase, and finally quantified for the external standard method under the multiple reaction monitoring (MRM) mode in the positive ionization scanning mode using electrospray ionization (ESI). The results showed that the limit of detection (LOD) of the SPE-UPLC-MS/MS method developed in this experiment was 25.0 ng/g for valnemulin and 5.0 ng/g for tiamulin. The correlation coefficient of linear calibration curve for valnemulin and tiamulin was over 0.99 within the concentration range 0.01 to 5.00 mug/mL. At the three supplemental levels (2.5, 25.0 and 125.0 mg/kg), the recovery for the valnemulin was between 85.17% and 94.55% and the relative standard deviation (RSD) was from 2.56% to 7.65%; the recovery for the tiamulin was between 84.69% and 99.36% and the RSD was from 1.57% to 4.95%. The results showed that the SPEUPLC-MS/MS method developed in this experiment is simple and sensitive, and it is fit for the rapid and quantitative determination of valnemulin and tiamulin in feed.
中文关键词	固相萃取 ; 超高效液相色谱-串联质谱 ; 饲料 ; 沃尼妙林 ; 泰妙菌素
英文关键词	solid phase extraction ultra performance liquid chromatography-tandem mass spectrometry feed valnemulin tiamulin
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:6260071
资源类型	期刊论文
条目标识符	http://119.78.100.177/qdio/handle/2XILL650/237506
作者单位	浙江大学饲料科学研究所, 浙江省饲料与动物营养重点实验室, 杭州, 浙江 310058, 中国
推荐引用方式 GB/T 7714	王凤芹,杨媛媛,陈楚昊,等. 固相萃取-超高效液相色谱-串联质谱法测定饲料中沃尼妙林和泰妙菌素[J],2018,30(6):2394-2401.
APA	王凤芹,杨媛媛,陈楚昊,胡喻涵,路则庆,&汪以真.(2018).固相萃取-超高效液相色谱-串联质谱法测定饲料中沃尼妙林和泰妙菌素.动物营养学报,30(6),2394-2401.
MLA	王凤芹,et al."固相萃取-超高效液相色谱-串联质谱法测定饲料中沃尼妙林和泰妙菌素".动物营养学报 30.6(2018):2394-2401.