超高效液相色谱-串联质谱法分析水及3种生物基质中矮壮素和野麦枯残留

Determination of chlormequat and difenzoquat in the blank water and bethree blank biological matrixes using ultra performance liquid chromatography-tandem mass spectrometry

建立了超高效液相色谱-串联质谱(UPLC-MS/MS)测定环境样品水基质以及人的血液、尿液和肝脏3种生物样品中矮壮素和野麦枯残留的方法。空白水、空白血、空白尿及空白肝脏样品中加入矮壮素和野麦枯标准溶液,经pH=8的氨水稀释后,涡旋离心,上清液过混合型弱阳离子交换柱(WCX)进行富集提取后,采用UPLC-MS/MS检测。质谱检测采用正离子扫描,多反应离子监测模式(MRM)。定性和定量均以矮壮素和野麦枯母离子和子离子进行分析。结果表明:试验期间矮壮素和野麦枯标准品在不同条件下的降解率为2.4%~11.9%,稳定性好。在0.010、0.10、0.25、0.50和1.0 mg/kg 5个添加水平下,矮壮素和野麦枯在空白水、空白血、空白尿及空白肝脏样品中的回收率在71%~104%之间,相对标准偏差在1.1%~19%之间,定量限均为0.01 mg/kg,检出限均为0.005 mg/kg。该方法灵敏度高,分析速度快,操作简便。

A method was developed for the quantitative determination and confirmation of chlormequat and difenzoquat using ultra performance liquid chromatography-tandem mass spectrometry(UPLCMS/MS). The blank water, blank whole blood, blank urine and blank liver were diluted by ammonia water(pH = 8), then vortexed and centrifuged. The supernatant was cleaned-up using Oasis?WCX solid phase extraction cartridges. Extracts was analyzed by UPLC-MS/MS in positive ionization and multiple reaction monitoring(MRM) mode. The parent ion and two daughter ions of chlormequat and difenzoquat were detected for quantification and confirmation. During the experiments, the degradation rates of standard products under different conditions ranged from 2.4% to 11.9%, and the stability was good. The recoveries of chlormequat and difenzoquat ranged from 71% to 110% with the spiked levels of 0.010, 0.10, 0.25, 0.50 and 1.0 mg/kg. And the relative standard deviation(RSD) ranged from 1.1%to 19%. The limits of quantification(LOQs) of all those herbicides were 0.01 mg/kg. The detection limit was 0.005 mg/kg. This method was proved to be selective, sensitive and rapid.