超高效液相色谱-串联质谱法测定动物组织中的金刚烷胺、金刚乙胺和盐酸美金刚

超高效液相色谱-串联质谱法测定动物组织中的金刚烷胺、金刚乙胺和盐酸美金刚
目的  建立超高效液相色谱-串联三重四极杆质谱法(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)测定动物组织中金刚烷胺、金刚乙胺和盐酸美金刚的分析方法。方法  样品经0.5%乙酸乙腈提取, 经过PCX固相萃取小柱净化, 以甲醇-含有0.1%甲酸的5 mmol/L乙酸铵水溶液为流动相, 经Agilent EclipsePlus C18 RRHD色谱柱, 进行梯度洗脱分离, 采用ESI正模式电离, 多反应监测(multiple reaction monitoring, MRM)模式进行检测, 以保留时间和定性离子对的相对丰度比定性, 内标法定量。结果  3种金刚烷胺类药物的检出限(limits of detection, LODs, S/N=3)和定量限(limits of quantitation, LOQs, S/N=10)分别为0.1 μg/kg和0.2 μg/kg, 在0.2~10 ng/mL浓度范围内, 线性关系良好(r2>0.999), 加标回收率为70.2%~ 82.7%, 相对标准偏差为3.9%~6.4%。结论  本方法操作简单、重现性好、背景噪音低、具有较高的灵敏度和选择性。

Objective  To establish a method for the determination of amantadine, rimantadine and memantine hydrochloride in animal tissue by ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods   The samples were extracted with a mixture of 0.5% acetic acid-acetonitrile and purified by PCX solid phase extraction column. The gradient elution program was applied in Agilent Eclipse Plus C18 RRHD column using the methanol-5 mmol/L ammonium acetate containing 0.1% formic acid as the mobile phase. The samples were analyzed by UPLC-MS/MS in positive electro spray ionization source (ESI) and multiple reaction monitoring (MRM) mode, the relative abundance ratio of retention time and qualitative ion was used for qualitative analysis, the internal standard method  was used for quantitative analysis. Results  The limits of detection (LODs, S/N=3) and limits of quantitation (LOQs, S/N=10) of 3 compounds were 0.1 μg/kg and 0.2 μg/kg, respectively. The linear relationship was good in the range of 0.2~10 ng/mL, and the correlation coefficients were more than 0.999. The recoveries were 70.2%~82.7%, and the relative standard deviations were in the range of 3.9%~6.4%. Conclusion  This method has the advantages of simple operation, good reproducibility, low background noise, and higher sensitivity and selectivity.

标题：超高效液相色谱-串联质谱法测定动物组织中的金刚烷胺、金刚乙胺和盐酸美金刚
英文标题：Determination of amantadine, rimantadine and memantine hydrochloride in animal tissue by ultra performance liquid chromatography-tandem  mass spectrometry

作者：
段科 青岛海润农大检测有限公司
刘刚 青岛海润农大检测有限公司
娄喜山 青岛海润农大检测有限公司
屠海云 青岛海润农大检测有限公司
刘亚飞 青岛海润农大检测有限公司
耿叙武 青岛海润农大检测有限公司

中文关键词:金刚烷胺,金刚乙胺,盐酸美金刚,超高效液相色谱-串联质谱法,
英文关键词:amantadine,rimantadine,memantine hydrochloride,ultra performance liquid chromatography- tandem mass spectrometry,

发表日期：2017-11-14

2025-1-31 19:54 上传 超高效液相色谱-串联质谱法测定动物组织中的金刚烷胺、金刚乙胺和盐酸美金刚.pdf

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