川芎嗪与12-钨磷酸相互作用的共振瑞利散射、二级散射和倍频散射光谱分析及其应用  

Resonance Rayleigh Scattering,Secondorder Scattering and Frequency Doubling Scattering Spectra of the Interaction for Tetramethylpyrazine with 12-Tungstophosphoric Acid and Its Analytical Applications

作　　者：杨金香[1] 李俊波[1] 杨小丽[1] 来丽娜[1] 

机构地区：[1]长治医学院药学系,山西长治046000

出　　处：《中国药学杂志》2014年第18期1642-1647,共6页Chinese Pharmaceutical Journal

基　　金：山西省高等学校科技创新项目资助(20121101)

摘　　要：目的建立测定川芎嗪的散射光谱新方法。方法在pH 1.5的HCl介质中,川芎嗪(TMP)与12-钨磷酸(TP)形成离子缔合物,在荧光分光光度计上以λex=λem进行同步扫描。结果离子缔合物的生成可引起共振瑞利散射(RRS)、二级散射(SOS)和倍频散射(FDS)光谱显著增强,其最大散射波长分别位于379、738和395 nm。在一定范围内,3种散射信号的增强(ΔIRRS,ΔISOS和ΔIFDS)均与川芎嗪的浓度呈线性关系。方法具有较高的灵敏度,共振瑞利散射,二级散射和倍频散射法对川芎嗪的检出限(3σ)分别为1.6,3.2和2.8 ng·mL-1。考察了适宜的反应条件和共存物质的影响,结果表明该方法选择性良好。结论提出了简便、快速、准确且高灵敏度的测定痕量川芎嗪的光散射新方法,应用于注射液和尿样中川芎嗪的测定,结果满意。OBJECTIVE To develop a new scattering spectra method for the determination of tetramethylpyrazine. METHODS In a HC1 medium （pH 1.5）, tetramethylpyrazine reacted with 12-tungstophosphorie acid to form a ion-association complexes, and the speetras of the system were recorded with synchronous scanning at λex=λem （ △λ = 0 nm）. RESULTS The intensities of resonance Rayleigh scattering （RRS）, second-order scattering （SOS） and frequency doubling cattering（FDS） were enhanced greatly and the new scattering spectra appeared. The maximum RRS, SOS and FDS wavelengths of three ion-association complexes were located at 379, 738 and 395 nm, respectively. The increments of scattering intensity （ΔIRRS,ΔISOS and ΔIFDS ） were directly proportional to the concentration of TMP in certain ranges. The detection limits （3σ） of TMP-TP system were 1.6 ng · mL^-1 （ RRS method）, 3.2 ng · mL^- 1 （ SOS method） and 2. 8 ng · mL^-1 （FDS method） , respectively. The optimum conditions of RRS method and the influence factors were discussed in the paper, in addition, the structure of ion-association complex and the reaction mechanism were investigated. CONCLUSION Based on the ion-association reaction and its spectral response, the rapid, simple and sensitive RRS method for the determination of TMP is been developed. It can be been applied to the determination of TMP in injection and urine samples with satisfactory results.

关 键 词：川芎嗪 12-钨磷酸 共振瑞利散射 二级散射 倍频散射 

分 类 号：R917[医药卫生—药物分析学]