固相萃取-高效液相色谱法测定水果蔬菜中的赤霉酸残留  

Detection of residual gibberellic acid(GA_3) in vegetables and fruits by the SPE-HPLC method

作　　者：史玉琴[1] 陈洪雨[1] 殷志萍[1] 王思思[1] 梁秋元[1] 赵文[1] 

机构地区：[1]河北农业大学食品科技学院,河北省农产品加工工程技术研究中心,河北保定071001

出　　处：《农药学学报》2011年第5期551-554,共4页Chinese Journal of Pesticide Science

基　　金：河北农业大学新兴学科科研发展项目(FSY200563)

摘　　要：采用固相萃取-高效液相色谱(SPE-HPLC)法建立了快速、准确检测果蔬中赤霉酸(GA3)残留量的方法。样本采用丙酮-水(5∶1,体积比)进行超声提取,经石油醚脱色、乙酸乙酯萃取、HyperSep C18固相萃取小柱净化(以1 mL甲醇为净化剂,以1 mL水为活化剂,上样液为1 mL 10%的甲醇,以5 mL 40%甲醇为洗脱剂),用HPLC检测,外标法定量。结果表明,GA3在0.05～10 mg/L范围内线性关系良好,相关系数r=0.999 7,检出限(LOD)为0.012 mg/kg。用所建立的方法抽检了18种市售果蔬样品,在1 mg/kg添加水平下的回收率在90.58%～99.35%之间,相对标准偏差在1.25%～8.67%之间。该方法稳定、准确,适用于果蔬中GA3的残留检测。A quick,accurate method to detect residual gibberellic acid（GA3） in fruits and vegetables by SPE-HPLC technique is established.GA3 was extracted by ultrasonic with acetone-water extractant（5∶4,V/V）;purified by discoloration of petroleum ether,extraction of ethyl acetate,and treatment of HyperSep C18 SPE column（column purification：1 mL methanol;column activator：1 mL water;sample absorption：1mL 10% methanol;eluent：5 mL neutral 40% methanol）;and finally detected by HPLC method,while its content was calculated by external standard method.The Results showed the method performed well within the linear range between 0.05 mg/L and 10 mg/L（r=0.999 7）,and the limit of detection was 0.012 mg/kg.The conducted spot check for 18 kinds of samples using the method showed that,the recovery rate was between 90.58% and 99.35% at the fortifed level of 1 mg/kg,while the RSD was between 1.25% and 8.67%,which indicated that the method was suitable for GA3 detection.

关 键 词：固相萃取 高效液相色谱 蔬菜和水果 赤霉酸 残留 

分 类 号：TQ452.12[化学工程—农药化工] O657.72[理学—分析化学]