摘要
目的采用气相色谱-质谱/质谱联用(GC-MS/MS)技术,建立了同时定性定量分析大米中环酰菌胺和啶酰菌胺药物残留量的方法。方法样品中的环酰菌胺和啶酰菌胺采用乙腈溶液提取,经无水硫酸镁及氯化钠盐析分层,提取液经无水硫酸镁、PSA吸附剂和C18固相吸附剂分散固相萃取净化,气相色谱-质谱/质谱检测和确证,外标法定量。结果环酰菌胺和啶酰菌胺线性良好,相关系数(r)均大于0.999 2,方法的最低检出限为0.01 mg/kg,啶酰菌胺回收率范围为70.3%~86.5%,相对标准偏差为5.98~8.51;环酰菌胺回收率范围为71.0%~89.0%,相对标准偏差为4.71~8.24。结论该方法具有选择性好、灵敏度高、回收率高、精密度好、操作简便等特点,适用于大米中环酰菌胺和啶酰菌胺药物残留量的测定。
Objective A method has been established to measure boscalid and fenhexamid in rice by GC-MS/ MS. Methods Boscalid and fenhexamid in rice were extracted with acetonitrile solution, and separated by anhydrous magnesium sulfate and sodium chloride. The extract was dispersed by anhydrous magnesium sulfate, PSA adsorbent and C18 solid phase adsorbent, phase extraction purification, gas chromatography-mass spectrometry/mass spectrometry (GC-MS/MS) detection and confirmation, external standard method for quantification. Results Cycloheximide and boscalid were linear, and the correlation coefficient (r) was greater than 0.999 2. The minimum detection limit of the method was 0.01 mg/kg, and the recovery rate of boscalid was from 70.3% to 86.5%. The relative standard deviation was from 5.98 to 8.51;the recovery rate of fenhexamid is from 71.0% to 89.0%, the relative standard deviation is from 4.71 to 8.24. Conclusion The method has the characteristics of good selectivity, high sensitivity, high recovery rate, good precision and simple operation, and is suitable for measuring the residual amount of fenhexamid and boscalid in rice.
作者
迟迅
赵韫慧
刘洋
修洋
宋清莲
顾婷婷
杨璐
胡婷婷
于海侠
CHI Xun;ZHAO Yunhui;LIU Yang;XIU Yang;SONG Qinglian;GU Tingting;YANG Lu;HU Tingting;YU Haixia(Changchun University of Chinese Medicine, Changchun 130117, China;Changchun Customs Technology Center, Changchun 130062, China;Changchun Anti-Cancer Pharmaceutical Research Institution, Changchun 130000, China)
出处
《长春中医药大学学报》
2019年第5期923-928,共6页
Journal of Changchun University of Chinese Medicine
基金
吉林省科技发展计划项目(20160309002YY)
