摘要
建立了切换检测波长同时测定葡萄组织中单体酚含量的高效液相色谱方法,使得全部待测物质能够在其最大吸收波长下得到检测。应用ZorbaxC18柱,以1.3%的乙酸水溶液和乙腈为流动相,梯度洗脱,流速0.8mL/min,柱温30℃。结果显示:各组分均得到很好分离,校准曲线的线性关系良好(r≥0.9990);平均加标回收率≥89.5%;保留时间及峰面积在日内(n=10)和日间(n=10)实验中的RSD分别≤0.3%、2.9%和0.3%、3.1%;与恒定检测波长的方法相比,该方法明显地降低了被测物质的检出限,并且在测定实际样品中得到了基线平稳、分离效果和峰形皆好的色谱图。该方法预处理简单、灵敏、重现性好。
A high performance liquid chromatographic method with switching detection wavelength was established for the simultaneous determination of individual phenolics in grape tissues. All phenolic compounds were detected under their maximal absorption wavelengths with a Zorbax C18column by gradient elution using CH3CN-1.3% CH3COOH as the mobile phase, the column temperature was controlled at 30℃ and the flow rate was 0.8 mL/min. The results showed that 6 phenolic compounds were separated well, and the linearity of calibration curves was good in the range of the test concentration (r ≥ 0. 9990 ). The average recoveries exceeded 89.5 % , and the relative standard deviations (RSD) of retention time and peak area in the inter-day (n = 10) tests and the intra-day (n = 10) ones were below 0.3%, 2.9% and 0.3%, 3.1%, respectively. Compared with the constant wavelength method, this method obviously reduced LOD and obtained stable-baseline, fine-separation, good-peak-shape chromatogram. The validated method has the advantages of simple pretreatment, sensitivity and good repeatability.
出处
《分析化学》
SCIE
EI
CAS
CSCD
北大核心
2007年第11期1614-1618,共5页
Chinese Journal of Analytical Chemistry
基金
国家重点成果推广项目(No2004EC000317)
西北农林科技大学青年学术骨干支持计划(No01140302)资助
关键词
高效液相色谱
切换波长
葡萄组织
单体酚
农药残留
High performance liquid chromatography, switching wavelength, grape tissues, individual phenolic