高效液相色谱-串联质谱法测定农产品中矮壮素残留量
HPLC-MS/MS Determination of Chlormequat in Agricultural Products
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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-10 mmol·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1.0~100 μg·L-1,检出限(3S/N)为5 μg·kg-1,测定下限(10S/N)为10 μg·kg-1.矮壮素在10,100,500 μg·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.Abstract: 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 1.0-100 μg·L-1,the detection limit (3S/N) was 5 μg·kg-1 and the quantitation limit was 10 μg·kg-1. Tests for recovery were made by addition of 10,100,500 μg·kg-1 of chlormequat,giving values of recovery in the range of 90.5%-98.5% and values of RSD′s (n=6) in the range of 0.99%-2.2%.