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采用批式进样分析与安培检测法对生物样品和膳食补充剂中的α-硫辛酸进行快速定量分析。

Fast quantification of α-lipoic acid in biological samples and dietary supplements using batch injection analysis with amperometric detection.

作者信息

Santos Pereira Laise Nayra Dos, da Silva Iranaldo Santos, Araújo Thaylan Pinheiro, Tanaka Auro Atsushi, Angnes Lúcio

机构信息

Departamento de Química, Universidade Federal do Maranhão, Avenida dos Portugueses, 1966, CEP 65080-805, São Luís, MA, Brazil.

Departamento de Química, Universidade Federal do Maranhão, Avenida dos Portugueses, 1966, CEP 65080-805, São Luís, MA, Brazil; Instituto Nacional de Ciência e Tecnologia de Bioanalítica, Caixa Postal 6154, CEP 13083-970 Campinas, SP, Brazil.

出版信息

Talanta. 2016 Jul 1;154:249-54. doi: 10.1016/j.talanta.2016.03.046. Epub 2016 Mar 15.

DOI:10.1016/j.talanta.2016.03.046
PMID:27154671
Abstract

Batch injection analysis (BIA) with amperometric detection, using a pyrolytic graphite electrode modified with cobalt phthalocyanine (PG/CoPc), was employed for determination of α-lipoic acid (ALA) in pharmaceutical product and in synthetic urine samples. The proposed BIA method is based on the application of a potential of +0.9V vs. Ag/AgCl, KCl sat, enabling quantification of ALA over a concentration range from 1.3×10(-6) to 1.0×10(-4)molL(-1), with a detection limit of 1.5×10(-8)molL(-1). A sampling rate of 180 injections per hour was attained and measurements of the reproducibility of successive injections (100µmolL(-1) ALA on the same electrode) showed a RSD of 2.11% for 40 successive injections. The new sensor was utilised for ALA quantification in a dietary pharmaceutical supplement and in synthetic urine and the results obtained for both samples were compared with parallel analysis using high performance liquid chromatography (HPLC), the method recommended by the United States Pharmacopeia. The results obtained were similar (at a 95% confidence level) and in the case of the synthetic urine sample (prepared with a known amount of ALA) the recovery was situated between 98.0% and 102.6%.

摘要

采用安培检测的批式进样分析(BIA),使用酞菁钴修饰的热解石墨电极(PG/CoPc),用于测定药品和合成尿液样品中的α-硫辛酸(ALA)。所提出的BIA方法基于相对于饱和KCl的Ag/AgCl施加+0.9V的电位,能够在1.3×10(-6)至1.0×10(-4)molL(-1)的浓度范围内对ALA进行定量,检测限为1.5×10(-8)molL(-1)。实现了每小时180次进样的采样率,对同一电极上连续进样(100µmolL(-1) ALA)的重现性测量显示,40次连续进样的相对标准偏差(RSD)为2.11%。该新型传感器用于膳食补充剂和合成尿液中ALA的定量分析,并将两个样品的分析结果与使用美国药典推荐的高效液相色谱(HPLC)的平行分析结果进行比较。获得的结果相似(在95%置信水平下),对于合成尿液样品(用已知量的ALA制备),回收率在98.0%至102.6%之间。

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