UV Spectrophotometric Determination of Trace Amounts of Doxycycline in Water with Separation and Enrichment by Gas Floatation
摘 要
水样中痕量的强力霉素(DXCC)用正丙醇及无水乙醇(4+1)作混合溶剂,从pH 8的溶液中进行气浮浮选使之分离并富集.加入氯化钠作为分相剂,加入铁(Ⅲ)使与DXCC反应生成憎水的络合物而浮选入有机相,在383 nm波长处测定有机相的吸光度.吸光度与DXCC浓度在3.1×10-7~2.0×10-5mol·L-1范围内呈线性关系,方法的检出限(3S/N)为2.6×10-7mol·L-1,测定中采用自制的气浮浮选装置.应用所提出的方法分析了3种不同来源的水样,并以此样品作为基体用标准加入法对方法的回收率进行了测定,测得方法的平均回收率为99.7%,测定值的相对标准偏差(n=5)均小于2.5%.
Abstract
Trace amounts of doxycycline (DXCC) in water sample were separated and enriched by gas floatation with hydrophilic solvent mixture of n-propanol and absolute alcohol(4+1),from a solution adjusted to pH 8 with 0.01 mol·L-1 NaOH solution.Sodium chloride was added as phase separating agent,and 1×10-4mol·L-1 Fe(NO3)3 solution was added to react with DXCC forming a hydrophobic complex,which was floated into the organic phase.Absorbance of the organic phase was measured photometrically at the wavelength of 383 nm.Linear relationship between values of absorbance and concentration of DXCC was obtained in the range of 3.1×10-7-2.0×10-5mol·L-1.Detection limit (3S/N) of the method found was 2.6×10-7mol·L-1.A self-made floutation installation was used in the determination.Samples of water from different sources were analyzed by the proposed method,and test for recovery was made by standard addition method using these samples as matrixes,giving values of average recovery of 99.7% and RSD′s (n=5) less than 2.5%.
中图分类号 O657.32
所属栏目 试验与研究
基金项目 国家自然科学基金项目(20777029);江苏省高校自然科学基础研究项目(07KJB610021),江苏大学研究生创新计划项目(CX07B-12X)
收稿日期 2008/8/11
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备注侯延民(1967-),男,河南汝州人,副教授,主要从事环境分析化学研究.
引用该论文: HOU Yan-min,YAN Yong-sheng,ZHAO Xiao-jun,WANG Liang. UV Spectrophotometric Determination of Trace Amounts of Doxycycline in Water with Separation and Enrichment by Gas Floatation[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2009, 45(4): 380~383
侯延民,闫永胜,赵晓军,王良. 气浮浮选分离富集-紫外分光光度法测定水中痕量强力霉素[J]. 理化检验-化学分册, 2009, 45(4): 380~383
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