Xu Dongpo, Liu Shaopu, Liu Zhongfang, Hu Xiaoli
School of Chemistry and Chemical Engineering, Southwest University, Chongqing 400715, PR China.
Anal Chim Acta. 2007 Apr 4;588(1):10-5. doi: 10.1016/j.aca.2007.01.076. Epub 2007 Feb 6.
A flow injection analysis (FIA) method coupled to resonance Rayleigh scattering (RRS) detection for the determination of verapamil hydrochloride (VP) was proposed. In pH 1.0 acidic medium, 12-tungstophosphoric acid (TP) reacted with VP to form an ion-association complex, which resulted in a significant enhancement of RRS intensity. The maximum scattering peak was located at 293 nm. RRS intensity was proportional to the concentration of VP in the range of 0.017-13.0 microg mL(-1), and the detection limit (3sigma) was 5.1 ng mL(-1). The proposed method exhibited satisfactory reproducibility with a relative standard derivation (R.S.D.) of 2.1% for 11 successive determinations of 5.0 microg mL(-1) VP. Therefore, a novel method for the determination of VP by FIA-RRS was developed. The optimum reaction conditions and the parameters of the FIA operation such as flow rate, injection volume, reactor length, and so on had been optimized in this paper. The present method had been applied to the determination of VP in serum samples and pharmaceuticals with satisfactory results. The maximal sample throughput in the optimized system was 80 h(-1).
提出了一种流动注射分析（FIA）法结合共振瑞利散射（RRS）检测来测定盐酸维拉帕米（VP）。在pH 1.0的酸性介质中，十二钨磷酸（TP）与VP反应形成离子缔合络合物，导致RRS强度显著增强。最大散射峰位于293 nm处。在0.017 - 13.0 μg mL⁻¹范围内，RRS强度与VP浓度成正比，检测限（3σ）为5.1 ng mL⁻¹。该方法具有良好的重现性，对5.0 μg mL⁻¹的VP连续11次测定的相对标准偏差（R.S.D.）为2.1%。因此，建立了一种用FIA - RRS测定VP的新方法。本文对最佳反应条件以及FIA操作参数如流速、进样体积、反应管长度等进行了优化。该方法已应用于血清样品和药物中VP的测定，结果令人满意。优化系统中的最大样品通量为80 h⁻¹。
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