分散固相萃取-HPLC-MS/MS法测定热带水果中4-氯苯氧乙酸

Determination of 4-Chlorophenoxyacetic Acid in Tropical Fruit by DSPE-HPLC-MS/MS

建立了分散固相萃取-高效液相色谱-串联质谱/质谱法测定热带水果中4-氯苯氧乙酸含量的方法,对方法的提取、净化和质谱条件进行了研究。方法采用1%乙酸-乙腈提取,以石墨化碳黑(GCB)作为净化剂分散固相萃取净化,液相色谱-质谱/质谱进行检测,外标法定量。检出限为0.3μg/kg。以热带水果为基质,当添加水平为1.0,10.0和100.0μg/kg时,回收率范围为81.0%~109.4%,相对标准偏差为2.7%~6.7%。经验证,该方法灵敏度、特异性和选择性均能满足热带水果中4-氯苯氧乙酸的检测要求。

A DSPE-HPLC-MS/MS method was developed for determining 4-Chlorophenoxyacetic acid in tropical fruit, and the conditions of extraction, purification and the mass spectrum were also discussed. 1% Acetic Acid-Acetonitrile was used as the extraction solvent, and GCB was used to purify. External standard method was used to quantify the target compounds with LC-MS/MS. The tested matrix was tropical fruit. The limits of detection were 0.3 μg/kg. Three spiked levels(1.0, 10.0 and 100.0 μg/kg) were applied, and the average recoveries and RSDs obtained were ranged from 81.0%-109.4% and 1.0%-6.7%, respectively. As proved, this method satisfied the requirements(including sensitivity, specificity and selectivity) of determining 4-Chlorophenoxyacetic acid in tropical fruit.