title: Rayleigh light scattering detection of three α1-adrenoceptor antagonists coupled with high performance liquid chromatograph.
abstract: Herein, a Rayleigh light-scattering (RLS) detection method combined with high performance liquid chromatograph (HPLC) without any post-column probe was developed for the separation and determination of three α₁-adrenoceptor antagonists. The quantitative analysis is benefiting from RLS signal enhancement upon addition of methanol which induced molecular aggregation to form an hydrophobic interface between aggregates and water that produce a sort of superficial enhanced scattering effect. A good chromatographic separation among the compounds was achieved using a Gemini 5u C₁₈ reversed phase column (250 mm × 4.6 mm; 4 μm) with a mobile phase consisting of methanol and ammonium acetate-formic acid buffer solution (25 mM; pH=3.0) at the flow rate of 0.7 mL min(-1). The RLS signal was monitored at λex=λem=354 nm. A limit of detection (LOD) of 0.065-0.70 μg L(-1) was reached and a linear range was found between peak height and concentration in the range of 0.75-15 μg L(-1) for doxazosin mesylate (DOX), 0.075-3.0 μg L(-1) for prazosin hydrochloride (PRH), and 0.25-5 μg L(-1) for terazosin hydrochloride (TEH), with linear regression coefficients all above 0.999. Recoveries from spiked urine samples were 88.4-99.0% which is within acceptable limits. The proposed method is convenient, reliable and sensitive which has been used successfully in human urine samples.
authors.affiliation: Chemistry and Chemical Engineering, Southwest University, Beibei District, Chongqing, PR China.
authors.forename: Ai Ping
authors.initials: AP
authors.lastname: Li
authors.affiliation: Chemistry and Chemical Engineering, Southwest University, Beibei District, Chongqing, PR China.
authors.forename: Huanjun
authors.initials: H
authors.lastname: Peng
authors.affiliation: Chemistry and Chemical Engineering, Southwest University, Beibei District, Chongqing, PR China. Electronic address: hxpengjd@swu.edu.cn.
authors.forename: Jing Dong
authors.initials: JD
authors.lastname: Peng
authors.affiliation: Chemistry and Chemical Engineering, Southwest University, Beibei District, Chongqing, PR China.
authors.forename: Ming Qiong
authors.initials: MQ
authors.lastname: Zhou
authors.affiliation: Chemistry and Chemical Engineering, Southwest University, Beibei District, Chongqing, PR China.
authors.forename: Jing
authors.initials: J
authors.lastname: Zhang
mesh_terms: D000317:Adrenergic alpha-Antagonists / Q000032:analysis / Q000652:urine*; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D019281:Dimerization; D017292:Doxazosin / Q000032:analysis / Q000652:urine*; D000067493:Dynamic Light Scattering / Q000379:methods*; D006801:Humans; D006860:Hydrogen Bonding; D057230:Limit of Detection; D008958:Models, Molecular; D011224:Prazosin / Q000031:analogs & derivatives* / Q000032:analysis / Q000652:urine*
chemical_list: D000317:Adrenergic alpha-Antagonists; C041226:Terazosin; D017292:Doxazosin; D011224:Prazosin
keywords: HPLC; Molecular aggregation; Rayleigh light-scattering; α(1)-Adrenoceptor antagonist