高效液相色谱串联质谱法测定玉米及植株中胺唑草酮及其代谢物

Determination of Amicarbazone and Its Metabolites in Corn and Its Plant with a Modified Qu ECh ERS by Liquid Chromatography-Tandem Mass Spectrometry

建立了同时测定玉米及玉米植株中胺唑草酮及其两个代谢物残留量的液相色谱串联质谱分析方法。样品采用乙腈提取,石墨化炭黑（GCB）和C18分散固相萃取净化,以甲醇-5 mmol/L乙酸铵溶液为流动相,液相色谱串联质谱分析测定。在1~1000μg/L的浓度范围内,3种目标化合物的响应值与浓度呈良好的线性关系,在3个添加水平下,玉米籽粒及植株中胺唑草酮及其代谢物的平均添加回收率为85%~111%,相对标准偏差（RSD）为2.3%~11.0%。方法定量限（LOQ）为5μg/kg。采用本方法监测15例市售玉米样品,样品中目标物均低于方法检出限。本方法简单,快速,灵敏度高,可完全满足国外胺唑草酮相关现行法规的限量要求。

A modified QuEChERS （Quick, Easy, Cheap, Effective, Rugged and Safe ） method was developed to analyze amicarbazone and its Metabolites residues in corn and its plant with liquid chromatography-tandem mass spectrometry （LC-MS/MS） detection. After extracted with MeCN and purified with graphite carbon black （GCB） and with Cls as dispersive solid phase extraction, the sample was measured by LC-MS/MS equipped an Agilent EC-Cls column with methanol-5 mmoL/L ammoniumaeetate as mobile phase. The linear range was 1-1000 μg/L and the recoveries ranged from 85.1%-111.0% with the relative standard deviations （RSDs） of 2.3 % - 11.0%. The limit of quantification （LOQ） was 5 μg/kg. The residues of amicarbazone （AMZ） and its metabolites （ DA and ISO） were lower than the limit of detection （LOQ） in 15 samples obtained from local markets. The results showed that the method was simple, fast, and efficient for analysis of amicarbazone and its metabolites in corn matrices.