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Simultaneous determination of amantadine and rimantadine in feed by liquid chromatography-Qtrap mass spectrometry with information-dependent acquisition
Analytical and Bioanalytical Chemistry ( IF 3.8 ) Pub Date : 2018-04-13 , DOI: 10.1007/s00216-018-1022-x
Qi Jia , Dan Li , Xinlu Wang , Shuming Yang , Yongzhong Qian , Jing Qiu

A sensitive method for simultaneous determination of amantadine and rimantadine in feed was developed using an ultra-high-performance liquid chromatography-triple quadrupole linear ion trap mass spectrometry (UHPLC-Qtrap-MS) in the multiple reaction monitoring information-dependent acquisition-enhanced product ion (MRM-IDA-EPI) mode, and employing the mixed cation exchange (MCX) solid-phase extraction column as sample cleanup and amantadine-d15 and rimantadine-d4 as internal standards, respectively. Compared to traditional MRM mode, for the targeted drugs in feed simultaneously both the secondary mass spectra and MRM information can be obtained using UHPLC-Qtrap-MS with MRM-IDA-EPI mode, and thus more accurate qualitative confirmation results achieved even at lower concentration of 0.2 μg/L in acceptable purity fit values. After optimization of sample preparation, good linearities (R > 0.9994) were obtained over the concentration range from 1 to 200 μg/L for amantadine and rimantadine. The precision was validated by intra-day and inter-day, and the relative standard deviations were all within 9.61%. Mean recoveries ranged from 76.1 to 112% at spiked concentrations of 0.5–100 μg/kg in three types of feed samples, including formula feed and complex concentrated feed for pigs and premix feed for chicken. The limits of detection (LODs) and quantification (LOQs) were 0.2 and 0.5 μg/kg for both drugs, respectively. The application in real feed samples further proved the accuracy and reliability of the developed method. This method provides an important tool to detect illegal uses of amantadine and rimantadine in feed.

Open image in new windowGraphical abstract
Graphical abstract

Simultaneous quantitation and qualitative confirmation of amantadine and rimantadine in feed by MRM-IDA-EPI



中文翻译:

信息相关采集-液相色谱-Qtrap质谱法同时测定饲料中的金刚烷胺和金刚烷胺

建立了一种同时测定饲料中金刚烷胺和金刚烷胺的灵敏方法,该方法用于多反应监测信息依赖型采集增强型产品中的超高效液相色谱-三重四极杆线性离子阱质谱(UHPLC-Qtrap-MS)离子(MRM-IDA-EPI)模式,并采用混合阳离子交换(MCX)固相萃取柱进行样品净化,并使用金刚烷胺d 15和金刚乙胺d 4作为内部标准。与传统的MRM模式相比,使用MRM-IDA-EPI模式的UHPLC-Qtrap-MS可以同时获得饲料中的目标药物的二级质谱图和MRM信息,因此即使在较低的浓度下也可以获得更准确的定性确认结果可接受的纯度拟合值为0.2μg/ L。优化样品制备后,良好的线性(R 金刚烷胺和金刚烷胺的浓度范围为1至200μg/ L,> 0.9994)。通过日内和日间验证精度,相对标准偏差均在9.61%以内。在三种饲料样品中,加标浓度为0.5–100μg/ kg时,平均回收率介于76.1%至112%之间,包括配方饲料和猪的复合浓缩饲料以及鸡的预混饲料。两种药物的检出限(LOD)和定量限(LOQ)分别为0.2和0.5μg/ kg。在实际饲料样品中的应用进一步证明了该方法的准确性和可靠性。该方法为检测饲料中金刚烷胺和金刚烷胺的非法使用提供了重要工具。

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图形概要

用MRM-IDA-EPI同时定量和定性测定饲料中的金刚烷胺和金刚烷胺

更新日期:2018-04-13
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