高效液相色谱法测定水性涂料中4种生物杀伤剂

水性涂料样品1.000g用约20 mL的1%(体积分数,下同)乙酸甲醇溶液超声提取20min,冷却至室温后,用1%乙酸甲醇溶液稀释至25.0mL,摇匀后,以2 000r·min^-1转速离心20min,上清液用0.45μm有机相过滤器过滤,采用高效液相色谱法测定滤液中多菌灵、敌草隆、百菌清和三氯生等4种生物杀伤剂的含量。以Agilent ZORBAX SB-C18色谱柱为分离柱,用甲醇和0.3%(体积分数)氨水以不同比例混合的溶液为流动相进行梯度洗脱,在检测波长236nm处进行测定。4种生物杀伤剂的质量浓度均在0.4~40.0mg·L^-1内与其对应的峰面积呈线性关系,检出限(3S/N)为0.47~1.10mg·kg^-1。加标回收率为92.5%~106%,回收量的相对标准偏差(n=7)为0.43%~2.8%。

HPLC Determination of 4 Biocides in Waterborne Coating

The waterborne coating sample(1.000 g)was extracted ultrasonically for 20 min with about20 mL of 1%(φ,the same below)acetic acid methanol solution.After cooling to room temperature,the solution was made up to 25.0 mL with 1%acetic acid methanol solution.After shaking up,the solution was centrifugated for20 min at the speed of 2 000 r·min^-1,and then the supernatant was filtered with 0.45μm organic phase filter.HPLC was applied to the determination of 4 biocides,i.e.carbendazim,diuron,chlorothalonil and triclosan in the filtrate.Agilent ZORBAX SB-C18 chromatographic column was used for separation with mixtures of methanol and0.3%(volume fraction)ammonia with different mixing ratios as mobile phase in the gradient elution.Detection at236 nm was adopted in the determination.Linear relationships between values of peak area and mass concentration of the 4 biocides were kept in the same range of 0.4-40.0 mg·L^-1,with detection limits(3 S/N)in the range of0.47-1.10 mg·kg^-1.Values of recovery found by standard addition method were in the range of 92.5%-106%,and values of RSDs(n=7)of recovery amounts were in the range of 0.43%-2.8%.