摘要
提出了微波消解样品,在线衍生测定疾藜提取物中痕量铅的反相高效液相色谱方法。双水杨醛邻苯二胺为衍生剂,用Diamonsil^(TM) C_(18)色谱柱(4.6 mm×150 mm,5μm)作为固定相,甲醇-水-衍生剂(64.5:34.0:1.5体积比)为流动相,检测波长为275 nm,柱温30℃。样品中铅在0.10～0.63 ng范围内呈线性,铅的平均回收率为99.5%,相对标准偏差(n=7)为1.8%。
In the method reported in this paper, microwave assisted sample digestion with HNO3 and HClO4 was adopted. Bis salicylaldehyde-o-phenyldiamine was used as derivatizing agent for Pb^2＋ ion. Diamonsil^TM C18 column （4. 6 mm×150 mm, 5 μm） was used as the stationary phase in the chromatographic separation. Methanol, water and bis-salicylaldehyde-o-phenyldiamine were mixed in the ratio of 64. 5 to 34. 0 to 1.5 by volume and the mixed solution was used as the mobile phase passing through the column at a flow-rate of 1. 1 mL · min^-1 , which was found to be proper for the on-line derivatization and for elution of the derivative. It was found that 30 ℃ was the suitable temperature for the column, and for UV-detection made at the wavelength of 275 nm. Linear relationship between values of peak area and amount of lead was obtained in the range 0. 10-0.63 ng. Average of recovery was found to be 99. 5%, with value of RSD＇s （n=7） to be 1.8%.
出处
《理化检验（化学分册）》
CAS
CSCD
北大核心
2008年第11期1021-1023,共3页
Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
基金
绵阳市科技局自然科学研究重点项目(06S041-04)
四川省教育厅重点项目(2005 A175)
关键词
高效液相色谱法
柱上衍生
铅(Ⅱ)
疾藜提取物
High performance liquid chromatography
On-column derivatization
Lead （Ⅱ）
Tribulus terrestris extract
