单嘧磺酯的HPLC/MS/MS研究  

Study on the Analysis of Monosulfuron-ester by HPLC/MS/MS

作　　者：蔡飞[1,2] 陈建宇[1,2] 王海英[1,2] 李正名[1,2] 

机构地区：[1]国家农药工程研究中心(天津),天津300071 [2]南开大学元素有机化学国家重点实验室,天津300071

出　　处：《农药学学报》2009年第3期388-391,共4页Chinese Journal of Pesticide Science

摘　　要：采用反相高效液相色谱和质谱联用技术(HPLC/MS),以电喷雾电离质谱(ESI/MS)和大气压化学电离质谱(APCI/MS),研究了单嘧磺酯的质谱特征。单嘧磺酯的ESI/MS正离子模式主要形成[M+H]+、[M+Na]+、[2M+Na]+、[2M+K]+等准分子离子峰和金属离子加合离子峰及二聚离子峰;ESI/MS负离子模式主要形成[M-H]-和[2M-2H+Na]-;单嘧磺酯质谱裂解形成的碎片离子得到了ESI多级质谱的证实。而APCI/MS主要形成[M+H]+、[M-H]-及与单嘧磺酯结构有关的碎片离子峰(m/z:110.31,136.24,168.18,244.19)。ESI/MS和APCI/MS负离子模式扫描形成明显的准分子离子峰且干扰小,可用于单嘧磺酯的结构表征和定性分析。APCI/MS正离子模式则有助于分析单嘧磺酯的碎片离子裂解方式。MS characteristics of monosulfuron-ester were analysized by comparison between reversed-phase HPLC/ESI/MS and HPLC/APCI/MS. Monosulfuron-ester gave positive-ion ESI/MS spectra with major [M＋H]＋ and [M＋Na]＋,[2M＋Na]＋,[2M＋K]＋ ion and negative-ion ESI-MS spectra with dominant [M-H]-and [2M-2H＋Na]-ions. Fragments and structurally informative spectra such as [M＋H]＋,[M-H]-and m/z of 110.31,136.24,168.18,244.19 were found in APCI/MS with [M＋H]＋ ion in positive-ion mode as predominant and [M-H]-ion in negative-ion mode as preferential.Accordingly,negative-ion of ESI/MS and APCI/MS could be utilized to identify monosulfuron ester by its molecular ions; whereas positive-ion of APCI/MS could be used for its identification study by the succeeding cleavage of the specific ions in multi MS/MS environment.

关 键 词：单嘧磺酯 电喷雾电离质谱 大气压化学电离质谱 

分 类 号：O657.63[理学—分析化学]