高效液相色谱法测定水性涂料中碘丙炔醇丁基氨甲酸酯

Determination of 3-iodo-2-propynylbutylcarbamate in water-borne coating material by high performance liquid chromatography

建立高效液相色谱法测定水性涂料中生物杀伤剂碘丙炔醇丁基氨甲酸酯的分析方法。1.00 g水性涂料样品用约8 mL的甲醇超声提取10 min,冷却至室温后,用甲醇稀释至10.0 mL,以20000 r/min转速离心5 min,上清液用0.22μm有机相滤膜过滤,采用高效液相色谱/二极管阵列检测器(HPLC/DAD)测定滤液中碘丙炔醇丁基氨甲酸酯的含量。以甲醇–0.05 mol/L磷酸二氢钾溶液(用磷酸调节pH至4.0±0.05)为流动相进行等度洗脱,采用Shim–pack GIST C_(18)色谱柱(250 mm×4.6 mm,5μm)分离,检测波长为230 nm。碘丙炔醇丁基氨甲酸酯的质量浓度在8.0~200.0μg/mL范围内与其对应的色谱峰面积线性关系良好,相关系数为0.9999,检出限为43 mg/kg。样品加标回收率为87.5%~99.6%,测定结果的相对标准偏差为1.36%~2.98%(n=6)。

A method for determining biocide 3-iodo-2-propynylbutylcarbamate(IPBC)in water–borne coating material by high performance liquid chromatography was established.1.00 g of water–borne coating material sample was extracted by ultrasonic for 10 min with about 8 mL methanol.After cooling to room temperature,the solution was diluted to 10.0 mL with methanol centrifugated for 5 min at the speed of 20000 r/min,the supernatant was filtered with 0.22μm organic phase filter,and the content of 3-iodo-2-propynylbutylcarbamate in the filtrate was determined by high performance liquid chromatography/diode array detector(HPLC/DAD).Shim–pack GIST C_(18) chromatographic column(250 mm×4.6 mm,5μm)was used for separation with methanol–0.05 mol/L potassium dihydrogen phosphate solution(adjusted the pH to 4.0±0.05 with phosphoric acid)as the mobile phase for isocratic elution.The detection wavelenth was 230 nm.The mass concentration of 3-iodo-2-propynylbutylcarbamate had a good linear relationship with its chromatographic peak area in the range of 8.0–200.0μg/mL,the correlation coefficient was 0.9999,and the detection limit was 43 mg/kg.The recovery rate of standard addition was 87.5%–99.6%,and the relative standard deviation of determination results was 1.36%–2.98%(n=6).