摘要
提出了农产品中矮壮素的高效液相色谱-串联质谱(HPLC-MS/MS)分析方法。样品经甲醇-水(1+1)溶液提取,正己烷液液萃取后,采用阳离子交换固相萃取柱净化。所得净化液以阳离子交换树脂与C18混合填料色谱柱为固定相,以含0.1%(体积分数)乙酸的乙腈-10mmol·L-1乙酸铵(1+1)溶液为流动相进行等度洗脱,采用电喷雾正离子源,多反应监测模式检测,同位素内标法定量。矮壮素的线性范围为1.0~100μg·L-1,检出限(3S/N)为5μg·kg-1,测定下限(10S/N)为10μg·kg-1。矮壮素在10,100,500μg·kg-1等3个加标水平的回收率为90.5%~98.5%之间,测定值的相对标准偏差(n=6)在0.99%~2.2%之间。
A method of HPLC-IMS/MS for determination of chlormequat in agricultural products was proposed.The sample was extracted with methanol-water(1+1)and hexane,and purified with a cation exchange solid-phase extraction column.The eluate was separated by isocratic elution using a mixed packing chromatogram column with cation exchange resin and C18 as stationary phase,and 10 mmol·L-1 ammonium acetate-acetonitrile solution containing 0.1%(φ)acetic acid as mobile phase.ESI+and MRM were adopted in MS/MS detection,and internal standard method was used for quantization.Linearity range of chlormequat was found between 1.0-100μg·L-1,the detection limit(3S/N)was 5μg·kg-1 and the quantitation limit was 10μg·kg-1.Tests for recovery were made by addition of 10,100,500μg·kg-1 of chlormequat,giving values of recovery in the range of90.5%-98.5% and values of RSD′s(n=6)in the range of 0.99%-2.2%.
出处
《理化检验（化学分册）》
CAS
CSCD
北大核心
2015年第3期336-339,共4页
Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
基金
中国检验检疫科学研究院基本科研资助项目(2012JK044)
