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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 establish a new method for the determination of tetramethylpyrazine by scattering spectroscopy. Methods Tetramethylpyrazine (TMP) and 12-tungstophosphoric acid (TP) formed an ion-association complex in pH 1.5 HCl medium and simultaneously scanned by λex = λem on a fluorescence spectrophotometer. As a result, the formation of ion-association complexes caused a significant enhancement of the RRS, SOS and FDS spectra with the maximum scattering wavelengths of 379, 738 and 395 nm, respectively. Within a certain range, the enhancement of three kinds of scattering signals (ΔIRRS, ΔISOS and ΔIFDS) showed a linear relationship with the concentration of ligustrazine. The detection limit (3σ) of tetramethylpyrazine by resonance Rayleigh scattering, second-order scattering and double-frequency scattering were 1.6, 3.2 and 2.8 ng · mL-1, respectively. The suitable reaction conditions and the influence of coexisting substances were investigated. The results show that the method has good selectivity. Conclusion A simple, rapid, accurate and sensitive method for the determination of trace ligustrazine by light scattering was proposed. The method was applied to the determination of ligustrazine in injection and urine samples with satisfactory results.