摘要
目的优化气相色谱串联质谱-内标法测定大米中杀虫环残留量。方法在甲酸酸性条件下,大米中杀虫环经甲醇提取浓缩后,通过N-丙基乙二胺(primary secondary amine,PSA)固相萃取小柱净化,用甲醇-二氯甲烷(1:99,V:V)洗脱,采用SH-Rxi-5Sil MS毛细管色谱柱分离,正离子模式电离,多反应监测(multiple reaction monitoring,MRM),内标法定量。结果杀虫环在0.05~1.00μg/m L范围内线性关系良好(r=0.9995),在0.10、0.20和0.80μg 3个浓度水平的平均加标回收率为91.0%~102.1%,相对标准偏差(relative standard deviation,RSD)在0.78%~3.63%之间。结论该方法操作简便,耗时较短,灵敏度高,重现性好,适用于大米中杀虫环残留的定性和定量测定。
Objective To optimize the gas chromatography tandem mass spectrometry-internal standard method for the determination of thiocyclam in rice. Method Under formic acid acidic conditions, thiocyclam in rice was extracted by methanol, purified by primary secondary amine（PSA） solid-phase extraction column, and eluted with methanol dichloromethane（1：99, V：V）. Thiocyclam was separated by SH-Rxi-5 Sil MS capillary gas chromatographic column, with electron ion source in positive mode and multiple reaction monitoring（MRM）, and quantified by inner standard solution. Results Thiocyclam showed a good linear relationship in the range from 0.05 to 1.00 μg/m L, and the correlation coefficient was 0.9995. The recoveries at 3 spiked levels（0.10, 0.20 and 0.80 μg） were 91.0%~102.1%, with the relative standard deviations（RSD） of 0.78%~3.63%. Conclusion This method is simple, convenient, sensitive and reproducible, which is suitable for the qualitative and quantitative determination of thiocyclam in rice.
出处
《食品安全质量检测学报》
CAS
2017年第12期4822-4826,共5页
Journal of Food Safety and Quality
关键词
大米
杀虫环
气相色谱串联质谱仪
内标
rice
thiocyclam
gas chromatography tandem mass spectrometry
intemal standard
