摘要
建立了一种同步检测稻田中硝磺草酮和2甲4氯残留的固相萃取-高效液相色谱-串联质谱(SPE-LC-MS/MS)分析方法。样品经乙酸乙酯提取后,用PSA吸附、C_(18)固相萃取小柱净化,C_(18)色谱柱分离,0.1%甲酸水-0.1%甲酸甲醇溶液为流动相,梯度洗脱分离,在电喷雾ESI离子源正、负离子模式下,采用质谱多反应监测(MRM)模式定性分析。结果表明:硝磺草酮和2甲4氯的检出限(LOD)分别为0.005和0.025 ng,定量限(LOQ)分别为0.01和0.05 mg/L。在0.001~2 mg/L和0.005~5 mg/L范围内,硝磺草酮和2甲4氯的质量浓度与对应的峰面积间呈良好的线性关系,其相关系数均大于0.999 7。在0.01~2 mg/L添加水平下,硝磺草酮在田水、土壤、植株、稻壳和糙米中的平均回收率为75%~103%,相对标准偏差(RSD)为0.1%~8.2%;在0.05~10 mg/L添加水平下,2甲4氯在田水、土壤、植株、稻壳和糙米中的平均回收率为90%~113%,RSD为0.5%~7.4%。说明该方法高效、快捷、精确度高,能够满足硝磺草酮和2甲4氯钠在稻田中的残留量检测分析要求。
A rapid multi-residue analytical method for the simultaneous determination of mesotrione and MCPA-Na was developed using dispersive solid phase extraction and high performance liquid chromatography-tandem mass spectrometry（SPE-LC-MS/MS）. The analytes were extracted by ethyl acetate, cleaned up by PSA and C_（18） solid phase extraction column, and separated on a reversed phase C_（18） column using a gradient elution program with 0.1% aqueous formic acid and 0.1% methanol formic acid as the mobile phase. Quantitative analysis was performed with electrospray ionization in positive/negative mode（ESI＋） /（ESI-） under multiple reaction monitoring（MRM） mode. In this study,the LODs of mesotrione and MCPA were 0.005 ng and 0.025 ng, respectively, and LOQ were 0.01 and0.05 mg/L, respectively. When the addition levels ranging from 0.001 to 2 mg/L mesotrione and from0.005 to 5 mg/L MCPA, there was a good linear relationship between the mass concentration and the corresponding peak area, and the correlation coefficients were higher than 0.9997. When the addition level ranged from 0.01 to 2 mg/L, the average recovery of mesotrione in water, paddy soil, rice plant,rice husk and brown rice was 75%-103%, and the relative standard deviation（RSD） ranged from 0.1% to 8.2%; when it ranged between 0.05-10 mg/L, the average recovery rate of MCPA in water, paddy soil, rice plant, rice husk and brown rice rate was between 90%-113%, and the RSD was between 0.5%-7.4%. Results indicated that this method is highly efficient, with good sensitivity and accuracy, which can meet the detection requirements of mesotrione and MCPA residues in Oryza sativa ecosystem samples.
作者
吴晓峰
欧晓明
金晨钟
梁骥
刘秀
李成业
孔玄庆
WU Xiaofeng OU Xiaoming JIN Chenzhong LIANG Ji LIU Xiu LI Chengye KONG Xuanqing(Collaborative Innovation Center for Field Weeds Control/Hunan University of Humanities, Science and Technology, Loudi 417000, Hunan Province, China Yongzhou Agricultural Science Research Institute, Yongzhou 425100, Hunan Province, China Hunan Research Institute of Chemical Industry/National Engineering Research Center for Agrochemicals/Hunan Provincial Key Laboratory of Agricultural Chemicals, Changsha 410000, Hunan Province, China)
出处
《农药学学报》
CAS
CSCD
北大核心
2017年第1期53-60,共8页
Chinese Journal of Pesticide Science
基金
湖南省高校产业化培育项目(13CY030)
湖南省高校创新平台开放基金项目(15K066)
湖南人文科技学院产学研合作引导项目(2013CXY04)
湖南省2015年研究生创新科研项目(CX2015B596)
关键词
固相萃取
高效液相色谱-串联质谱
硝磺草酮
2甲4氯钠
残留
稻田
solid-phase extraction
high performance liquid chromatography-tandem mass spectrometry（HPLC-MS/MS）
mesotrione
MCPA-Na
residue
rice ecosystem
