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固相萃取-高效液相色谱法测定水果蔬菜中的赤霉酸残留
引用本文:史玉琴,陈洪雨,殷志萍,王思思,梁秋元,赵文.固相萃取-高效液相色谱法测定水果蔬菜中的赤霉酸残留[J].农药学学报,2011,13(5):551-554.
作者姓名:史玉琴  陈洪雨  殷志萍  王思思  梁秋元  赵文
作者单位: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
基金项目: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。

关 键 词:固相萃取    高效液相色谱    蔬菜和水果    赤霉酸    残留
收稿时间:2011/5/14 0:00:00
修稿时间:2011/8/22 0:00:00

Detection of residual gibberellic acid (GA3) in vegetables and fruits by the SPE-HPLC method
SHI Yu-qin,CHEN Hong-yu,YIN Zhi-ping,WANG Si-si,LIANG Qiu-yuan and ZHAO Wen.Detection of residual gibberellic acid (GA3) in vegetables and fruits by the SPE-HPLC method[J].Chinese Journal of Pesticide Science,2011,13(5):551-554.
Authors:SHI Yu-qin  CHEN Hong-yu  YIN Zhi-ping  WANG Si-si  LIANG Qiu-yuan and ZHAO Wen
Institution:1.College of Food Science and Technology,Agricultural University of Hebei,Engineering Technology Research Center for Agricultral Product processing of Hebei,Baoding 071001,China
Abstract: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.
Keywords:gibberellic acid(GA3)  SPE  HPLC  fruits and vegetables  residue
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