烟草科技
煙草科技
연초과기
TOBACCO SCIENCE & TECHNOLOGY
2015年
1期
54-58
,共5页
郭卫芸%边照阳%唐纲岭%李中皓%杨飞%王建龙
郭衛蕓%邊照暘%唐綱嶺%李中皓%楊飛%王建龍
곽위예%변조양%당강령%리중호%양비%왕건룡
超高效合相色谱%四溴菊酯%溴氰菊酯%烟草
超高效閤相色譜%四溴菊酯%溴氰菊酯%煙草
초고효합상색보%사추국지%추청국지%연초
Ultra performance convergence chromatography (UPC2)%Tralomethrin%Deltamethrin%Tobacco
为实现烟草中四溴菊酯和溴氰菊酯的同时分析,利用QuEChERS前处理方法萃取烟草样品并对萃取液进行初步净化,采用弗罗里硅土固相萃取小柱对萃取液作进一步净化处理,采用超高效合相色谱仪(非极性的HSS C18 SB色谱柱作固定相,甲醇为流动相辅助剂)检测了四溴菊酯和溴氰菊酯。结果表明:四溴菊酯和溴氰菊酯残留量的分析可在6.5 min内完成,线性范围均为0.5~25.0 mg/kg,相关系数(R2)大于0.9995,平均加标回收率分别为92.6%和84.3%,相对标准偏差均小于10%,定量限分别为0.33和0.23 mg/kg。该方法弥补了气相色谱法不能检测四溴菊酯的不足。
為實現煙草中四溴菊酯和溴氰菊酯的同時分析,利用QuEChERS前處理方法萃取煙草樣品併對萃取液進行初步淨化,採用弗囉裏硅土固相萃取小柱對萃取液作進一步淨化處理,採用超高效閤相色譜儀(非極性的HSS C18 SB色譜柱作固定相,甲醇為流動相輔助劑)檢測瞭四溴菊酯和溴氰菊酯。結果錶明:四溴菊酯和溴氰菊酯殘留量的分析可在6.5 min內完成,線性範圍均為0.5~25.0 mg/kg,相關繫數(R2)大于0.9995,平均加標迴收率分彆為92.6%和84.3%,相對標準偏差均小于10%,定量限分彆為0.33和0.23 mg/kg。該方法瀰補瞭氣相色譜法不能檢測四溴菊酯的不足。
위실현연초중사추국지화추청국지적동시분석,이용QuEChERS전처리방법췌취연초양품병대췌취액진행초보정화,채용불라리규토고상췌취소주대췌취액작진일보정화처리,채용초고효합상색보의(비겁성적HSS C18 SB색보주작고정상,갑순위류동상보조제)검측료사추국지화추청국지。결과표명:사추국지화추청국지잔류량적분석가재6.5 min내완성,선성범위균위0.5~25.0 mg/kg,상관계수(R2)대우0.9995,평균가표회수솔분별위92.6%화84.3%,상대표준편차균소우10%,정량한분별위0.33화0.23 mg/kg。해방법미보료기상색보법불능검측사추국지적불족。
In order to analyze the tralomethrin and deltamethrin in tobacco simultaneously, the extract was preliminarily purified after tobacco sample was extracted by QuRChERS pretreatment, the extract was further purified with Florisil solid phase extraction column. Tralomethrin and deltamethrin were determined by ultra performance convergence chromatography (UPC2) with non-polar HSS C18 SB column as solid phase and methanol as mobile phase auxiliary agent. The results showed that it only took 6.5 minutes to complete the analysis of tralomethrin and deltamethrin residues, the linear range of this method were 0.5-25.0 mg/kg with the correlation coefficient (R2) more than 0.999 5 and relative standard deviation less than 10%. The average standard addition recoveries and detection limits of tralomethrin and deltamethrin were 92.6%, 84.3% and 0.33, 0.23 mg/kg, respectively. This method advantages over gas chromatography, the later fails to detect tralomethrin.