共振光散射光谱法测定异烟肼的含量  被引量:5

Determination of Isoniazid by Resonance Light Scattering Spectrometry Based on Ion-Association Reaction

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作  者:朱梦[1,2] 李倩 牟城健[1,2] 马卫兴 ZHU Meng;LI Qian;MOU Chengjian;MA Weixing(l.School of Chemical Engineering,Huaihai Institute of Technology,Lianyungang 222005,Chin;School of Pharmacy,Huaihai Institute of Technology,Lianyungang 222005,China;J iangsu Provincial Key Laboratory for Marine Pharmaceutical Screening,Lian yungang 222005,China)

机构地区:[1]淮海工学院化学工程学院,连云港222005 [2]淮海工学院药学院,连云港222005 [3]江苏省海洋药物筛选重点试验室,连云港222005

出  处:《理化检验(化学分册)》2018年第9期1035-1038,共4页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基  金:淮海工学院研究生科研创新计划项目(XKY-CXX2017-15)

摘  要:在10mL比色管中,加入5.00×10-4 mol·L-1三氯化铁溶液0.60mL和适量的异烟肼样品溶液,微波加热2min,冷却至室温后依次加入5.00×10-3 mol·L-1碘化钾溶液1.00mL、1.00×10-4 mol·L-1十六烷基三甲基溴化铵溶液0.30mL,用水稀释至10mL,静置20min后于荧光分光光度计上,在激发波长和发射波长均为275nm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0.050~0.25mg·L-1内与ΔI呈线性关系,检出限(3s/k)为0.015mg·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%。An appropriate amount of isoniazid sample solution and 0.60 mL of 5.00×10-4 mol·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 5.00×10-3 mol·L-1 potassium iodide solution was added and mixed well,0.30 mL of 1.00×10-4 mol·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,andΔI=I0-I was calculated.Linear relationship was found between ΔI and mass concentration of isoniazid in the range of0.050-0.25 mg·L-1,with detection limit(3 s/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 than2.0%.

关 键 词:异烟肼 共振光散射光谱法 离子缔合反应 

分 类 号:O657.3[理学—分析化学]

 

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