流动注射化学发光法测定丁香酚

Flow Injection Analysis of Eugenol with Chemiluminescent Detection

发现丁香酚对鲁米诺 二甲亚砜 氢氧化钠化学发光体系的抑制作用 ,在此基础上首次建立了测定丁香酚的化学发光分析法。该法灵敏度高、线性范围宽、操作简单 ,测定丁香酚的线性范围为 5× 10 -9～ 1× 10 -6g/mL ,检出限为 2 .97× 10 -9g/mL (S/N =3) ,对 5× 10 -7g/mL的丁香酚标准溶液进行 11次平行测定 ,相对标准偏差 (RSD)为 1.6 3%。该法用于中药丁桂儿脐贴中丁香酚的测定 ,其回收率为 93.3%～ 98.3% ,结果令人满意。通过对化学发光光谱、紫外可见吸收光谱的研究 ,提出其抑制作用机理可能是丁香酚与鲁米诺竞争消耗由二甲亚砜 氢氧化钠 O2 体系产生的O· -2 。

Eugenol is main chemical component of flos caryophylli dry bud from eugenia caryophyllata thunb. It has several biological roles, including sterilization function, antioxidation and narcotism. It has been widely used in food and medicine. The detection of eugenol is of considerable interests for food and pharmaceutical analysis. To date, a number of methods such as gas chromatography, gas chromatography/mass spectrometry, high-performance liquid chromatography, thin layer chromatography and spectrophotometry has been reported. However, former four methods required expensive instrumentation and tedious sample pretreatment and last method suffered from lower sensitivity. Therefore, it is necessary to explore new sensitive and simple method for the determination of eugenol. In this work, it was found that eugenol inhibited strongly the chemiluminescence of luminol-DMSO-NaOH system. On this basis, a novel flow injection method with inhibited chemiluminescent detection was developed. The optimal conditions for the detection of eugenol are as follows: 6.0×10^(-4) mol/L pH 8.00 luminol, 0.5 mol/L DMSO,0.1 mol/L NaOH. The method is sensitive, fast, and simple, superior to all documented methods. It allows for the detection of eugenol in the range of 5×10^(-9)～1×10^(-6) g/mL with a detection limit of 2.97×10^(-9)g/mL. The relative standard deviation is 1.63 % for the determination of 5×10^(-7)g/mL eugenol (n=11). The method has been successfully used to determine eugenol in traditional Chinese medicine ding erqi tie with the recoveries of 93.3%~98.3% and the results obtained by this method were comparable with that by gas chromatography. Finally, the CL spectra and UV-visible absorption spectra were studied and the CL inhibition mechanism has been proposed due to the competition of eugenol with luminol for O^(·-)_2 generated by DMSO-NaOH-O_2 system.