弱阴离子超高交联树脂固相萃取-高效液相色谱-紫外法测定人尿中高香草酸的含量

建立了人体尿液中高香草酸含量的固相萃取-高效液相色谱-紫外测定方法.合成了弱阴离子超高交联树脂固相萃取填料,并对其进行吸附性能考察.利用此萃取剂对尿液中的高香草酸进行选择性吸附,洗脱液富集后以甲醇-乙酸(15∶85,V/V)溶液为流动相,C18为固定相,于280 nm测定其中的高香草酸.方法验证结果表明,高香草酸在2.26～145 mg/L浓度范围内呈良好的线性关系；检出限为0.45 mg/L;方法的平均加标回收率大于90％；RSD小于4.2％.采用本方法对8名健康人尿样中的高香草酸含量进行了测定,结果为1.55～6.79 mg/L.表明本方法选择性好、灵敏度高、准确可靠.

Determination of Homovanilic Acid in Human Urine by Weak Anion Exchange Hypercrosslinked Polymer Resin-SPE-HPLC-UV method

A solid phase extraction-high performance liquid chromatography method with ultraviolet visible detector was developed for the determination of homovanilic acid(HVA) in human urine.Firstly,the hypercrosslinked resins modified with weak anion group were synthesized as solid phase extract packing material,and the adsorption performance was investigated.Then the homovanilic acid in urine was selectively absorbed on this absorbent.After elution,the homovanilic acid in enriched eluent was analyzed on a C18 column with the mobile phase of methanol and acetic acid solution(15 ∶ 85,V/V) and detection wavelength of 280 nm.The method validation results demonstrated that good linearity was obtained from 2.26 mg/L to 289 mg/L HVA and the limit of detection was 0.45 mg/L.The average recoveries were above 90% and RSD values were lower than 4.2%.The method was successfully applied to determinate the HVA contents of eight healthy human urines ranging from 1.55 mg/L to 6.79 mg/L.The results showed that the proposed method was highly selective,sensitive,accurate,and reliable.