提出了高效液相色谱法测定海洋涂料中的吡啶硫酮锌含量的方法。涂料样品(0.020 0 g)用乙酸乙酯(10 mL)超声提取10 min。取上清液5 mL,加入0.5 mol·L-1硝酸铜溶液5 mL进行衍生化。以Agilent ZORBAX Eclipse XDB-C18色谱柱为分离柱,用乙腈和水以不同体积比的混合液为流动相进行梯度洗脱,用二极管阵列检测器在检测波长242 nm处进行测定。吡啶硫酮锌的质量浓度在0.25~200 mg·L-1范围内与其峰面积呈线性关系,检出限(3S/N)为14 mg·kg-1。在3个浓度水平进行加标回收试验,回收率在89.3%~92.9%之间,测定值的相对标准偏差(n=6)均小于3.0%。

A method of HPLC for the determination of ZnPT in marine paint was proposed. The sample (0.020 0 g) was extracted for 10 min ultrasonically with ethyl acetate (10 mL). An aliquot of 5 mL of the supernatant was derivatized with 5 mL of 0.5 mol·L-1 Cu(NO3)2 solution. Agilent ZORBAX Eclipse XDB-C18 chromatographic column with mixtures of acetonitile and water with different mixing ratios as mobile phase in the gradient elution. UV-detection with DAD at 242 nm was adopted in the determination. Linear relationship between values of peak area and mass concentration of ZnPT was kept in the range of 0.25-200 mg·L-1 with detection limit (3S/N) of 14 mg·kg-1. Tests for recovery were made by standard addition method at 3 concentration levels, giving values of recovery in the range of 89.3%-92.9% with RSD′s (n=6) less than 3.0%.