干旱区生态环境知识资源中心(Arid): 超高效液相色谱-电喷雾串联质谱法测定猪尿中金刚烷胺与金刚乙胺的残留量

Arid

	超高效液相色谱-电喷雾串联质谱法测定猪尿中金刚烷胺与金刚乙胺的残留量
其他题名	Simultaneous Determination of Amantadine and Rimantadine Residues in Swine Urine by LC - MS/MS
	胡丽芳; 张金艳; 罗林广
来源期刊	分析测试学报
ISSN	1004-4957
出版年	2014
卷号	33 期号:6 页码:678-682
中文摘要	采用超高效液相色谱-电喷雾串联质谱(UPLC-ESI-MS/MS)在多反应监测(MRM)模式下建立了猪尿中金刚烷胺和金刚乙胺残留量的检测方法。尿样经乙腈超声提取,Oasis MCX固相萃取柱净化后,使用 Eclipse Plus C_(18)柱(RRHD 1.8 mum, 2. 1 mm * 100 mm)进行分离,以甲醇-0. 1%甲酸水溶液作为流动相进行梯度洗脱,电喷雾正离子(ESI~+)模式电离,多反应监测(MRM)模式进行定性定量测定。色谱保留时间和质谱碎片的离子丰度比定性,内标法定量。结果表明,2种待测物在0.2~20.0 mug/L范围内线性关系良好,相关系数(r~2)均大于0.999,该方法测得在猪尿样液中,金刚烷胺和金刚乙胺的检出限(LOD)均为0.05 mug/L,定量下限(LOQ)均为0.2 mug/L;平均加标回收率为89.7% ~ 102.8%,日内相对标准偏差为2. 8% ~4. 2%。
英文摘要	A rapid determination method for amantadine and rimantadine in swine urine was established using ultra performance liquid chromatography - electrospray tandem mass spectrometry (UPLC - ESI-MS/MS) in multiple reaction monitoring (MRM) mode. The urine sample was extracted with acetonitrile by ultrasonic, and cleaned up with solid-phase extraction Oasis MCX column. The separation of compounds was carried on an Eclipse Plus C_(18) (RRHD 1.8 mum, 2. 1 mm * 100 mm) by gradient elution using methanol -0. 1% formic acid as mobile phase. The electrospray was operated in the positive mode and the samples were monitored under the multiple reaction monitoring (MRM) mode. The chromatographic retention time and mass fragment ion abundance ratio were taken for qualitative confirmation, and the internal standard method was employed for quantification analysis. The limits of detection (LOD) for both compounds were 0. 05 mug/L, and the limits of quantitation (LOQ) were 0. 2 mug/L in swine urine. The correlation coefficients of the swine urine were greater than 0. 999 (r~2 >0. 999) within 0. 2 - 20. 0 mug/L linear ranges. Recoveries of amantadine and rimantadine at spiked levels of 0. 5 -20. 0 mug/L were in the range of 89. 7% - 102. 8% with intra-day relative standard deviation(RSDs) of 2. 8% -4. 2%.
中文关键词	超高效液相色谱-电喷雾串联质谱法(UPLC-ESI-MS/MS) ; 金刚烷胺 ; 金刚乙胺 ; 猪尿
英文关键词	ultra performance liquid chromatography - electrospray tandem mass spectrometry (UPL C - ESI - MS/MS) amantadine rimantadine swine urine
语种	中文
国家	中国
收录类别	CSCD
WOS类目	CHEMISTRY ANALYTICAL ; PHARMACOLOGY PHARMACY
WOS研究方向	Chemistry ; Pharmacology & Pharmacy
CSCD记录号	CSCD:5175000
资源类型	期刊论文
条目标识符	http://119.78.100.177/qdio/handle/2XILL650/231034
作者单位	江西省农业科学院农产品质量安全与标准研究所农产品质量安全重点实验室, 南昌, 江西 330200, 中国
推荐引用方式 GB/T 7714	胡丽芳,张金艳,罗林广. 超高效液相色谱-电喷雾串联质谱法测定猪尿中金刚烷胺与金刚乙胺的残留量[J],2014,33(6):678-682.
APA	胡丽芳,张金艳,&罗林广.(2014).超高效液相色谱-电喷雾串联质谱法测定猪尿中金刚烷胺与金刚乙胺的残留量.分析测试学报,33(6),678-682.
MLA	胡丽芳,et al."超高效液相色谱-电喷雾串联质谱法测定猪尿中金刚烷胺与金刚乙胺的残留量".分析测试学报 33.6(2014):678-682.