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
4期
1117-1124
,共8页
史晓梅%陈士恒%章晴%杨永坛
史曉梅%陳士恆%章晴%楊永罈
사효매%진사항%장청%양영단
六六六%滴滴涕%分散固相萃取%气相色谱法%大米
六六六%滴滴涕%分散固相萃取%氣相色譜法%大米
륙륙륙%적적체%분산고상췌취%기상색보법%대미
hexachlorocyclohexane%dichlorodiphenyltrichloroethane%dispersive solid phase extraction%gas chromatography%rice
目的：建立气相色谱-电子捕获检测器法(GC-ECD)测定大米中六六六和滴滴涕(α-六六六、β-六六六、γ-六六六、δ-六六六、o,p’-滴滴滴、o,p’-滴滴伊、o,p’-滴滴涕、p,p’-滴滴滴、p,p’-滴滴伊、p,p’-滴滴涕)残留量的方法。方法大米样品经乙腈超声提取后,应用PSA进行分散固相萃取净化,高速离心后氮吹浓缩定容,最后使用气相色谱电子捕获检测器测定。结果六六六和滴滴涕在0.002~0.1 mg/L 浓度范围内呈现良好线性关系, R2大于0.99；在0.002、0.005、0.01 mg/kg三个添加浓度上回收率范围为84.10%~111.43%,相对标准偏差小于9.23%,检出限在0.0001~0.0007 mg/kg之间。结论该方法前处理操作快速简单,重复性好且灵敏度高,满足国内外对大米中六六六和滴滴涕快速、准确检测的要求,可应用于大量样品的定性定量分析。
目的：建立氣相色譜-電子捕穫檢測器法(GC-ECD)測定大米中六六六和滴滴涕(α-六六六、β-六六六、γ-六六六、δ-六六六、o,p’-滴滴滴、o,p’-滴滴伊、o,p’-滴滴涕、p,p’-滴滴滴、p,p’-滴滴伊、p,p’-滴滴涕)殘留量的方法。方法大米樣品經乙腈超聲提取後,應用PSA進行分散固相萃取淨化,高速離心後氮吹濃縮定容,最後使用氣相色譜電子捕穫檢測器測定。結果六六六和滴滴涕在0.002~0.1 mg/L 濃度範圍內呈現良好線性關繫, R2大于0.99；在0.002、0.005、0.01 mg/kg三箇添加濃度上迴收率範圍為84.10%~111.43%,相對標準偏差小于9.23%,檢齣限在0.0001~0.0007 mg/kg之間。結論該方法前處理操作快速簡單,重複性好且靈敏度高,滿足國內外對大米中六六六和滴滴涕快速、準確檢測的要求,可應用于大量樣品的定性定量分析。
목적：건립기상색보-전자포획검측기법(GC-ECD)측정대미중륙륙륙화적적체(α-륙륙륙、β-륙륙륙、γ-륙륙륙、δ-륙륙륙、o,p’-적적적、o,p’-적적이、o,p’-적적체、p,p’-적적적、p,p’-적적이、p,p’-적적체)잔류량적방법。방법대미양품경을정초성제취후,응용PSA진행분산고상췌취정화,고속리심후담취농축정용,최후사용기상색보전자포획검측기측정。결과륙륙륙화적적체재0.002~0.1 mg/L 농도범위내정현량호선성관계, R2대우0.99；재0.002、0.005、0.01 mg/kg삼개첨가농도상회수솔범위위84.10%~111.43%,상대표준편차소우9.23%,검출한재0.0001~0.0007 mg/kg지간。결론해방법전처리조작쾌속간단,중복성호차령민도고,만족국내외대대미중륙륙륙화적적체쾌속、준학검측적요구,가응용우대량양품적정성정량분석。
Objective To develop a method for the simultaneous determination of hexachlorocyclohexane (HCH) and dichlorodiphenyltrichloroethane (DDT) (α-HCH, β-HCH, γ-HCH, δ-HCH, o,p’-DDD, o,p’-DDE, o,p’-DDT, p,p’-DDD, p,p’-DDE, p,p’-DDT) residues in rice by gas chromatography with ECD detector using dispersive solid phase extraction. Methods Rice samples were extracted with acetonitrile assisted by ul-tra-sonic, and the extracts were purified by dispersive solid phase extraction using PSA as the purification sor-bent. After high speed centrifugation and concentrated by nitrogen flushing, samples were detected by GC-ECD. Results The method showed a good linearity in the range of 0.002~0.1 mg/L for HCH and DDT with R2>0.99. The recoveries were in the range of 84.10%~111.43% at three spiked levels of 0.002, 0.005, 0.01 mg/kg for HCH and DDT, and the relative standard deviations (RSDs) were less than 9.23%. The limits of detections were in the range of 0.0001~0.0007 mg/kg. Conclusion The method is suitable for quantitative and qualita-tive analysis of HCH and DDT in a sufficient number of rice samples with sensitivity and repeatability, and which could meet the fast and accurate detection requirements of HCH and DDT residues testing at home and abroad.
