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
8期
2488-2495
,共8页
谢建军%李菊%陈捷%席静%陈文锐%李敏青
謝建軍%李菊%陳捷%席靜%陳文銳%李敏青
사건군%리국%진첩%석정%진문예%리민청
气相色谱-质谱联用法%固相分散萃取%农药%残留检测
氣相色譜-質譜聯用法%固相分散萃取%農藥%殘留檢測
기상색보-질보련용법%고상분산췌취%농약%잔류검측
gas chromatography-mass spectrometry%solid-phase dispersion%pesticide%residue detection
目的:建立固相分散萃取结合气相色谱-质谱联用法(GC/MS)快速测定葡萄酒中敌敌畏、乐果、二嗪磷等葡萄种植过程中常用43种杀虫剂、杀螨剂及杀菌剂残留量。方法样品用乙腈快速提取、氯化钠和无水硫酸镁盐析后,经 GCB粉、NH2粉和 PSA粉组合吸附剂净化, GC/MS外标法定性定量。结果43种农药在10~500μg/L范围内线性关系良好,相关系数R2在0.9851~0.9997范围内,空白添加浓度在50~200μg/kg时,其回收率在67.43%~114.74%之间,相对标准差(n=6)小于13.6%,方法的测定下限(LOD)介于1~50μg/kg 之间。结论本法简单、准确、快速,适合于葡萄酒中对43种农药残留量的检测。
目的:建立固相分散萃取結閤氣相色譜-質譜聯用法(GC/MS)快速測定葡萄酒中敵敵畏、樂果、二嗪燐等葡萄種植過程中常用43種殺蟲劑、殺螨劑及殺菌劑殘留量。方法樣品用乙腈快速提取、氯化鈉和無水硫痠鎂鹽析後,經 GCB粉、NH2粉和 PSA粉組閤吸附劑淨化, GC/MS外標法定性定量。結果43種農藥在10~500μg/L範圍內線性關繫良好,相關繫數R2在0.9851~0.9997範圍內,空白添加濃度在50~200μg/kg時,其迴收率在67.43%~114.74%之間,相對標準差(n=6)小于13.6%,方法的測定下限(LOD)介于1~50μg/kg 之間。結論本法簡單、準確、快速,適閤于葡萄酒中對43種農藥殘留量的檢測。
목적:건립고상분산췌취결합기상색보-질보련용법(GC/MS)쾌속측정포도주중활활외、악과、이진린등포도충식과정중상용43충살충제、살만제급살균제잔류량。방법양품용을정쾌속제취、록화납화무수류산미염석후,경 GCB분、NH2분화 PSA분조합흡부제정화, GC/MS외표법정성정량。결과43충농약재10~500μg/L범위내선성관계량호,상관계수R2재0.9851~0.9997범위내,공백첨가농도재50~200μg/kg시,기회수솔재67.43%~114.74%지간,상대표준차(n=6)소우13.6%,방법적측정하한(LOD)개우1~50μg/kg 지간。결론본법간단、준학、쾌속,괄합우포도주중대43충농약잔류량적검측。
Objective A rapid analytical method was developed for the determination of 43 pesticide residues in grape wine by solid-phase dispersion with gas chromatography-mass spectrometry (GC/MS). Methods Toally 43 pesticide residues were extracted from the samples with acetonitrile, and then detected by GC/MS with external standard method after being cleaned up with three sorbents (PSA 80.0 mg、GCB 30.0 mg and NH2 30.0 mg). Results Good linearities of 10?500μg/L were obtained and correlation coefficients were 0.9851?0.9997. The recoveries of all pesticides were in the range from 67.43%to 114.74%at the spiked levels of 50, 100, and 200μg/kg in grape wine, and the relative standard deviations (RSDs) were not more than 13.6%. The limits of detection (LOD) were 1~50μg/kg. Conclusion The method could be used for the determination of 43 pesticide residues in grape wine due to its simpleness, accuracy and rapidness.