食品安全质量检测学报
食品安全質量檢測學報
식품안전질량검측학보
FOOD SAFETY AND QUALITY DETECTION TECHNOLOGY
2014年
9期
2871-2878
,共8页
袁烁%赵建庄%蔡慧敏%贾临芳%梁丹%魏朝俊
袁爍%趙建莊%蔡慧敏%賈臨芳%樑丹%魏朝俊
원삭%조건장%채혜민%가림방%량단%위조준
草莓%固相萃取%气相色谱法%农药残留
草莓%固相萃取%氣相色譜法%農藥殘留
초매%고상췌취%기상색보법%농약잔류
strawberry%solid-phase extraction%gas chromatography%pesticide residues
目的:建立一种固相萃取-毛细管柱气相色谱方法,可以同时检测草莓中常用的13种农药残留,包括百菌清、腐霉利、粉唑醇、腈菌唑、醚菌酯、苯醚甲环唑、烯酰吗啉等7种杀菌剂,毒死蜱、三氟氯氰菊酯、哒螨灵、氰戊菊酯等4种杀虫剂及莠去津、乙草胺等2种除草剂。方法草莓样品20 g匀浆后,经乙腈50 mL提取, NH2固相萃取柱净化, HP-5毛细管气相色谱柱进行分离, GC-ECD 进行定性及定量分析。结果13种农药残留的色谱图分离效果良好,线性相关系数均大于0.996,方法检出限在0.01 mg/kg~0.5 mg/kg之间。13种农药的添加水平为0.01 mg/kg~2 mg/kg,回收试验表明该方法平均回收率在70.5%~114.5%之间,相对标准偏差在2.17%~6.85%之间。结论该方法简单、快速、灵敏、净化效果好、回收率高,适合草莓中多种农药残留的检测和安全监控。通过对50份草莓样品进行检测,检出百菌清、乙草胺、毒死蜱、粉唑醇、醚菌酯、烯酰吗啉6种农药。
目的:建立一種固相萃取-毛細管柱氣相色譜方法,可以同時檢測草莓中常用的13種農藥殘留,包括百菌清、腐黴利、粉唑醇、腈菌唑、醚菌酯、苯醚甲環唑、烯酰嗎啉等7種殺菌劑,毒死蜱、三氟氯氰菊酯、噠螨靈、氰戊菊酯等4種殺蟲劑及莠去津、乙草胺等2種除草劑。方法草莓樣品20 g勻漿後,經乙腈50 mL提取, NH2固相萃取柱淨化, HP-5毛細管氣相色譜柱進行分離, GC-ECD 進行定性及定量分析。結果13種農藥殘留的色譜圖分離效果良好,線性相關繫數均大于0.996,方法檢齣限在0.01 mg/kg~0.5 mg/kg之間。13種農藥的添加水平為0.01 mg/kg~2 mg/kg,迴收試驗錶明該方法平均迴收率在70.5%~114.5%之間,相對標準偏差在2.17%~6.85%之間。結論該方法簡單、快速、靈敏、淨化效果好、迴收率高,適閤草莓中多種農藥殘留的檢測和安全鑑控。通過對50份草莓樣品進行檢測,檢齣百菌清、乙草胺、毒死蜱、粉唑醇、醚菌酯、烯酰嗎啉6種農藥。
목적:건립일충고상췌취-모세관주기상색보방법,가이동시검측초매중상용적13충농약잔류,포괄백균청、부매리、분서순、정균서、미균지、분미갑배서、희선마람등7충살균제,독사비、삼불록청국지、달만령、청무국지등4충살충제급유거진、을초알등2충제초제。방법초매양품20 g균장후,경을정50 mL제취, NH2고상췌취주정화, HP-5모세관기상색보주진행분리, GC-ECD 진행정성급정량분석。결과13충농약잔류적색보도분리효과량호,선성상관계수균대우0.996,방법검출한재0.01 mg/kg~0.5 mg/kg지간。13충농약적첨가수평위0.01 mg/kg~2 mg/kg,회수시험표명해방법평균회수솔재70.5%~114.5%지간,상대표준편차재2.17%~6.85%지간。결론해방법간단、쾌속、령민、정화효과호、회수솔고,괄합초매중다충농약잔류적검측화안전감공。통과대50빈초매양품진행검측,검출백균청、을초알、독사비、분서순、미균지、희선마람6충농약。
Objective To established a solid phase extraction-capillary gas chromatography method for the determination of 13 pesticides multi-residues in strawberry, including seven fungicides such as chlorothalonil, procymidone, flutriafol, myclobutanil, kresoxim-methyl, difenoconazole and dimethomorph;four insecticides such as chlorpyrifos, cyhalothrin, pyridaben and fenvalerate;two herbicides such as atrazine and acetochlor. Methods After the homogenized strawberry samples with 20 g were extracted with acetonitrile by 50 mL and purified with NH2 solid-phase extraction column, the samples were separated by HP-5 gas chromatography column and detected with GC-ECD. Results A good separation for 13 pesticides was achieved using the established method, with correlation coefficients above 0.996. The detection limit of the method was 0.01~0.5 mg/kg. Shown as the addition recovery experiments, the method average recoveries of the 13 pesticides ranged from 70.5% to 114.5% in the range of 0.01 mg/kg~2 mg/kg. The relative standard deviation was 2.17%~6.85%. Conclusion The method showed simple, rapid, and sensitive, with good purifying effect and high recovery rate, and was suitable for the detection and security monitoring of pesticide residues in strawberry. Six kinds of pesticides, chlorothalonil, chlorpyrifos, acetochlor, flutriafol, kresoxim methyl, and dimethomorph, were found through the detection in 50 strawberry samples.