Determination of Isoniazid by Resonance Light Scattering Spectrometry
摘 要
在10 mL比色管中,加入5.00×10-4mol·L-1三氯化铁溶液0.60 mL和适量的异烟肼样品溶液,微波加热2 min,冷却至室温后依次加入5.00×10-3mol·L-1碘化钾溶液1.00 mL、1.00×10-4mol·L-1十六烷基三甲基溴化铵溶液0.30 mL,用水稀释至10 mL,静置20 min后于荧光分光光度计上,在激发波长和发射波长均为275 nm处测量溶液的散射强度I,同时测量空白溶液的散射强度I0,计算ΔI=I0-I。异烟肼的质量浓度在0.050~0.25 mg·L-1内与ΔI呈线性关系,检出限(3s/k)为0.015 mg·L-1。方法应用于异烟肼片的分析,测定值与标示量相符,测定值的相对标准偏差(n=6)小于2.0%。
Abstract
An appropriate amount of isoniazid sample solution and 0.60 mL of 5.00×10-4mol·L-1 ferric chloride solution were added into a 10 mL colorimetric tube. The tube was heating by microwave for 2 min, and cooled to room temperature. Then 1.00 mL of 5.00×10-3mol·L-1 potassium iodide solution was added and mixed well, 0.30 mL of 1.00×10-4mol·L-1 cetyltrimethylammonium bromide solution was added and mixed well. After the mixed solution was diluted to 10 mL with water, and allowed to stand for 20 min, the scattering intensity (I) of the solution was measured at both the excitation wavelength and the emission wavelength of 275 nm, using a fluorescence spectrophotometer. The scattering intensity (I0) of the blank solution was measured, and ΔI=I0-I was calculated. Linear relationship was found between ΔI and mass concentration of isoniazid in the range of 0.050-0.25 mg·L-1, with detection limit (3s/k) of 0.015 mg·L-1. The proposed method was applied to analysis of isoniazid tablets, giving measured values consistent with the labeled values, and RSDs (n=6) less than 2.0%.
中图分类号 O657.3 DOI 10.11973/lhjy-hx201809009
所属栏目 工作简报
基金项目 淮海工学院研究生科研创新计划项目(XKY-CXX2017-15)
收稿日期 2017/10/18
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备注朱梦,硕士研究生,研究方向为药物分析
引用该论文: ZHU Meng,LI Qian,MOU Chengjian,MA Weixing. Determination of Isoniazid by Resonance Light Scattering Spectrometry[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2018, 54(9): 1035~1038
朱梦,李倩,牟城健,马卫兴. 共振光散射光谱法测定异烟肼的含量[J]. 理化检验-化学分册, 2018, 54(9): 1035~1038
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【3】BARSOUM N B, KAMEL M S, DIAB M M A. Spectrophotometric determination of isoniazid and rifampicin from pharmaceutical preparations and biological fluids[J]. Research Journal of Agricultural and Biological Sciences, 2008,4(5):471-484.
【4】NAGARAJA P, MURTHY K C S, YATHIRAJAN H S. Spectrophotometric determination of isoniazid with sodium 1,2-naphthoquinone-4-sulphonate and cetyltrimethyl ammonium bromide[J]. Talanta, 1996,43(7):1075-1080.
【5】CHELLINI P R, LAGESE B, FRANCO P H C, et al. Development and validation of an HPLC method for simultaneous determination of rifampicin, isoniazid, pyrazinamide, and ethambutol hydrochloride in pharmaceutical formulations[J]. Journal of AOAC International, 2015,98(5):1234-1239.
【6】AYYAPPAN J, UMAPATHI P, QUINE S D. Development and validation of a stability indicating high-performance liquid chromatography (HPLC) method for the estimation of isoniazid and its related substances in fixed dose combination of isoniazid and ethambutol hydrochloride tablets[J]. African Journal of Pharmacy and Pharmacology, 2011,5(12):1513-1521.
【7】SABITHA P, RATNA J V, REDDY K R. A new RP-HPLC method for the determination of isoniazid in plasma[J]. Drug Invention Today, 2010,2(7):331-334.
【8】LAPA R A S, LIMA J L F C, SANTOS J L M. Fluorimetric determination of isoniazid by oxidation with cerium (IV) in a multicommutated flow system[J]. Analytica Chimica Acta, 2000,419(1):17-23.
【9】KOHNO H, KUBO H, FURUKAWA K, et al. Fluorometric determination of isoniazid and its metabolites in urine by high-performance liquid chromatography using in-line derivatization[J]. Therapeutic Drug Monitoring, 1991,13(5):428-432.
【10】ABSALAN G, AKHOND M, SOLEIMANI M, et al. Efficient electrocatalytic oxidation and determination of isoniazid on carbon ionic liquid electrode modified with electrodeposited palladium nanoparticles[J]. Journal of Electroanalytical Chemistry, 2016,761:1-7.
【11】CHEN W C, UNNIKRISHNAN B, CHEN S M. Electrochemical oxidation and amperometric determination of isoniazid at functionalized multiwalled carbon nanotube modified electrode[J]. International Journal of Electrochemical Science, 2012,7(10):9138-9149.
【12】KHUHAWAR M Y, ZARDARI L A. Capillary gas chromatographic determination of isoniazid in pharmaceutical preparations and blood by precolumn derivatization with trifluoroacetylacetone[J]. Journal of Food and Drug Analysis, 2006,14(4):323-328.
【13】盛若虹.间接原子吸收光谱法测定异烟肼的含量[J].光谱实验室, 2010,27(1):331-334.
【14】BI S, WANG Y, PANG B, et al. Study on naringenin-CTMAB-DNA system by resonance light scattering technique and its analytical application[J]. Spectrochimica Acta Part A:Molecular and Biomolecular Spectroscopy, 2011,79(5):1430-1434.
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