HPLC法测定人体尿液样品中的4'-羟基黄烷酮和6-甲氧基黄烷酮

报道一种快速测定人体尿液中4'-羟基黄烷酮和6-甲氧基黄烷酮的HPLC方法.采用自制的大蒜新素键合硅胶填充柱(DTSP,4.6 mm i.d.×15 mm,10 μm),以乙腈/1.5%三乙胺-甲酸(65:35,v/v,pH=3.0) 为流动相,流速设定为1.0 mL·minn~(-1),检测波长为 257 nm时,实现了人体尿样品中上述黄烷酮化合物的良好分离.4'-羟基黄烷酮的线性范围为5～100 mg·L~(-1),r=0.992 0;6-甲氧基黄烷酮线性范围为5～100 mg·L~(-1),r=0.999 1,它们的最低检出限分别为1.03 ng和1.56 ng,平均回收率分别为99.02%～99.26%和98.21%~98.62%,相应的RSD分别小于0.354%和0.605%(n=5).该方法快速、简便、可靠,适用于人体尿液样品中上述黄烷酮分离分析.

Determination of 4'-hydroxyflavanoneand 6-methoxyflavanone in Human Urine Samples by HPLC

A rapid analytical method of determinating 4'-hydroxyflavanone and 6 - methoxyflavanone in human urine samples by HPLC. Baseline separation was carried out on a home-made allitridin bonded silica gel packed column with acetonitrile/1.5%TEA-HCOOH buffer(65:35,v/v,pH=3)as mobile phase at a flow rate of 1.0 mL·minn~(-1).The detection wavelength was at 257nm.The two kinds of flavanones in human urine were separated. The linear ranges and the correlation coefficient of 4'-hydroxyflavanone and 6-methoxylflavanone were 5～100 mg·L~(-1)(r=0.9920) and 5～100mg·L~(-1),(r=0.9991).The average recoveries from spiked human urine samples were 99.02%～99.26% (RSD<0.354%,n=5)and 98.21%～98.62% (RSD<0.605%,n=5),and their minimum detection limit were 1.03 ng,1.56 ng,respectively.The method is rapid,simple and reliable for the determination of the above flavanones in human urines.