三氟乙酰丙酮衍生试剂毛细管气相色谱法测定脑脊液中γ-氨基丁酸和Putrescine

IF 0.4 Q4 CHEMISTRY, ANALYTICAL Pakistan Journal of Analytical & Environmental Chemistry Pub Date : 2018-06-27 DOI:10.21743/PJAEC/2018.06.02
L. A. Zardari, M. A. Kamboh, Hamid Rashidi Nodeh, A. Laghari, M. Y. Khuhawar, S. Khokhar
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引用次数: 0

摘要

在气相色谱-火焰离子化检测器(GC-FID)分析脑脊液(CSF)样品之前,用三氟乙酰丙酮(FAA)作为衍生试剂测定γ氨基丁酸(GABA)和腐胺(Put)。GABA, Put,尸胺(Cad)和酪胺(TY)作为FAA的模拟物,从HP-5柱(30 m x 0.32 mm i.d)中提取,温度为110℃,持续1分钟,加热速率为25℃至260℃/min。采用FID进行检测,分离比为10:1,v/v,整个运行时间为10 min。该方法的线性校准范围为2.5-50µg/mL,低检出限为1.0 - 2.5µg/mL,与所选Put, Cad, GABA,采用预浓缩法测定人脑脊液中GABA和Put的含量,分别为0.25 ~ 0.56µg/mL和0.16 ~ 0.41µg/mL,相对标准偏差(RSD)分别为0.8 ~ 1.1和1.1 ~ 1.5%。许多氨基酸的测试,完全分离,并没有改变测定的GABA和Put。
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Capillary Gas Chromatographic Determination of Gamma Aminobutyric acid and Putrescine in Cerebrospinal Fluid using Trifluoroacetylacetone as Derivatizing Reagent
determination of gamma aminobutyric acid (GABA) and putrescine (Put) using trifluoroacetylacetone (FAA) as derivatizing reagent from Cerebrospinal Fluid (CSF) samples prior to their gas chromatographic- flame ionization detector (GC-FID) analysis. GABA, Put, cadaverine (Cad) and tyramine (TY) as imitative of FAA extracted from the column HP-5 (30 m x 0.32 mm i.d) at temperature 110 oC for 1 min, tracked by heating rate 25 oC to 260 oC /min. The detection was carried out by FID with segregate ratio 10:1, v/v with whole run time 10 min. The proposed method showed linear calibration range between 2.5-50 µg/mL with low limit of detection 1.0 - 2.5 µg/mL analogous to 0.1 ng to 0.25 ng for selected Put, Cad, GABA, and TY. The method based on the pre-concentration was used for the determination of GABA and Put from CSF of human being and amounts found were 0.25- 0.56 µg/mL and 0.16 - 0.41 µg/mL with relative standard deviation (RSD) within 0.8 - 1.1 and 1.1 - 1.5 %, respectively. Many of aminoacids tested, separated completelyand did not variate the determinations of GABA and Put.
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CiteScore
1.10
自引率
16.70%
发文量
16
审稿时长
15 weeks
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