分析科学学报
分析科學學報
분석과학학보
JOURNAL OF ANALYTICAL SCIENCE
2009年
6期
634-638
,共5页
陈良壁%曾景斌%赵瑨云%王翊如%陈曦
陳良壁%曾景斌%趙瑨雲%王翊如%陳晞
진량벽%증경빈%조진운%왕익여%진희
固相微萃取%农残检测%气相色谱
固相微萃取%農殘檢測%氣相色譜
고상미췌취%농잔검측%기상색보
Solid-phase microextraction%Pesticides%Gas chromatography%Vegetables
通过合成羟基聚甲基苯基硅氧烷(PMPS-OH)材料,制备固相微萃取(SPME)纤维涂层.通过与商品化聚二甲基硅氧烷(PDMS)、聚丙烯酸酯(PA)和PDMS/聚二乙烯基苯(DVB)纤维对六六六异构体(α,β,γ,δ-BHC)、DDT及其衍生物(p,p′-DDD,p,p′-DDE,o,p′-DDT,p,p′-DDT)、联苯菊酯、甲氰菊酯、高效氟氯氰菊酯、三氟氯氰菊酯、氯氰菊酯和氰戊菊酯等选定农药萃取效果的比较,所制备的PMPS-OH纤维具有更好的萃取效率.对SPME实验条件进行了研究和优化,测定方法对各种农药的线性范围多在0.01~2 ng/g之间,相应的检出限在0.001~0.05 ng/g范围,回收率在50.5%~103%.方法已被应用于蔬菜样品中农残的检测.
通過閤成羥基聚甲基苯基硅氧烷(PMPS-OH)材料,製備固相微萃取(SPME)纖維塗層.通過與商品化聚二甲基硅氧烷(PDMS)、聚丙烯痠酯(PA)和PDMS/聚二乙烯基苯(DVB)纖維對六六六異構體(α,β,γ,δ-BHC)、DDT及其衍生物(p,p′-DDD,p,p′-DDE,o,p′-DDT,p,p′-DDT)、聯苯菊酯、甲氰菊酯、高效氟氯氰菊酯、三氟氯氰菊酯、氯氰菊酯和氰戊菊酯等選定農藥萃取效果的比較,所製備的PMPS-OH纖維具有更好的萃取效率.對SPME實驗條件進行瞭研究和優化,測定方法對各種農藥的線性範圍多在0.01~2 ng/g之間,相應的檢齣限在0.001~0.05 ng/g範圍,迴收率在50.5%~103%.方法已被應用于蔬菜樣品中農殘的檢測.
통과합성간기취갑기분기규양완(PMPS-OH)재료,제비고상미췌취(SPME)섬유도층.통과여상품화취이갑기규양완(PDMS)、취병희산지(PA)화PDMS/취이을희기분(DVB)섬유대륙륙륙이구체(α,β,γ,δ-BHC)、DDT급기연생물(p,p′-DDD,p,p′-DDE,o,p′-DDT,p,p′-DDT)、련분국지、갑청국지、고효불록청국지、삼불록청국지、록청국지화청무국지등선정농약췌취효과적비교,소제비적PMPS-OH섬유구유경호적췌취효솔.대SPME실험조건진행료연구화우화,측정방법대각충농약적선성범위다재0.01~2 ng/g지간,상응적검출한재0.001~0.05 ng/g범위,회수솔재50.5%~103%.방법이피응용우소채양품중농잔적검측.
Hydroxyl-terminated polymethylphenylsiloxane (PMPS-OH) was synthesized and successfully used as a novel coating for solid-phase microextraction (SPME). PMPS-OH coated fiber was applied to the analysis of pesticides including α,β,γ,δ-BHC,p,p′-DDD, p,p′-DDE, o,p′-DDT, p,p′-DDT, bifenthrin, fenpropathrin, β-cyfluthrin, cyhalothrin, cypermethrin and fenvalerate by SPME-GC-ECD. The extraction efficiencies of the PMPS-OH coated fiber for selected pesticides were found to be higher than those of commercial fibers, such as PDMS, PA and PDMS/DVB. The SPME experimental conditions including stirring rate, extraction temperature and time, were studied, and the optimal conditions were established. The linearity for the target pesticides was from 0.01 to 2 ng/g, and the detection limits were between 0.001 and 0.05 ng/g. The proposed approach was applied to the determination of pesticides in vegetable samples, and the recovery for the pesticides spiked in vegetables at 4 ng/g ranged from 50.5% to 103%.