在线光纤传感同步吸收-荧光光谱检测仪测定阿司匹林片中游离水杨酸

Online optical fiber sensing synchronous absorption-fluorescence spectrum detector determination of the free salicylic acid in aspirin

目的 建立在线光纤传感同步吸收-荧光光谱法测定阿司匹林中游离水杨酸的方法 。方法 采用在线光纤传感同步吸收-荧光光谱法测定不同厂家阿司匹林片中水杨酸,1%冰醋酸-甲醇溶液作为溶剂,20%甲醇作为载液,泵流速1.00 m L/min,进样体积50μL时,300 nm为吸收波长,303 nm为激发波长,430 nm为发射波长进行检测。结果 游离水杨酸在0.5～5.0μg/m L（r=0.9994）范围内线性良好。拜阿司匹林、阿司匹林肠溶片、阿司匹林泡腾片中游离水杨酸的平均加样回收率分别为98.01%、98.32%、98.40%;精密度、稳定性、重复性的RSD均〈1.60%。结论 该方法灵敏度高、重复性好,适用于阿司匹林中游离水杨酸的检测。

Objective To establish an online optical fiber sensing Synchronous absorption-fluorescence spectrometer for detection of free salicylic acid in aspirin. Methods Free salicylic acid in aspirin from different manufacturer was measured by online optical fiber sensing synchronous absorption - fluorescence spectrometry, as soon as solvent was 1% glacial acetic acid - methanol solution, carrying fluid was 20% methanol, pump flow rate was 1.00 mL/min, sample volume was 50 μL, 300 nm was selected absorption wavelength, 303 nm was selected fluorescence excitation wavelength, 430 nm was selected emission wavelength to be proceeded. Results The linear ranges of free salicylic acid was 0.5-5.0 μg/mL （r=0.9994）. The average recovery of free salicylic acid in aspirin, aspirin enteric tablets and aspirin effervescent tablets were 98.00%1 98.32%, 98.40%; the RSD of precision, stability, repeatability were less than 1.60%. Conclusion The method is high sensitivity and good repeatability for the residue analysis of free salicylic acid in aspirin.