超高效液相色谱-串联质谱法测定水稻糙米和植株中盐酸吗啉胍残留

Determination of Moroxydine Hydrochloride Residue in Brown Rice and Plant by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

【目的】建立超高效液相色谱-串联质谱法（UPLC—MS／MS）测定水稻糙米和植株基质中盐酸吗啉胍残留量。【方法】水稻糙米和植株经三氯乙酸振荡提取，用OasisHLB或C18固相萃取小柱净化，采用UPLC-MS／MS正离子扫描测定残留的盐酸吗啉胍。【结果】糙米和植株的3种添加质量分数（0．05、0．5、3．0mg／kg）的平均回收率分别为93．6％-105．4％和92．5％～109．2％，相对标准偏差分别为2．6％～7.2％和6．1％-7．7％。在糙米和植株中的检出限为0．005mg／kg。【结论】该方法操作简单，灵敏度高，定量准确，可用于水稻糙米和植株中盐酸吗啉胍残留分析。

[Aims] A method for the confirmation and quantification of moroxydine hydrochloride residues in brown rice and plant was established based on ultra performance liquid chromatography-tandem mass spectrometry （UPLC-MS/MS）. [Methods] Brown rice and plant were extracted with trichloroacetic acid, cleaned up by Oasis HLB or C,s SPE cartridge column. The detection was performed by tandem mass spectrometry with electrospray ionization in positive mode （ESI＋）. [Results] Average recoveries of brown rice at three spiked levels （0.05, 0.5 and 3.0 mg/kg） were found in the range of 93.6- 105.4% with RSD of 2.6-7.2%. Average recoveries of plant at three spiked levels （0.05, 0.5 and 3.0 mg/kg） were found in the range of 92.5-109.2% with RSD of 6.1-7.7%. Limits of detection （LOD） of brown rice and plant were 0.005 mg/kg. [Conclusions] The method is sample and suitable for routine and confirmation analysis of moroxydine hydrochloride.