福建分析测试
福建分析測試
복건분석측시
FUJIAN ANALYSIS & TESTING
2013年
6期
28-31,36
,共5页
陈志涛%姜晖%郑香平%赵建晖%陈春添%林荆
陳誌濤%薑暉%鄭香平%趙建暉%陳春添%林荊
진지도%강휘%정향평%조건휘%진춘첨%림형
固相萃取%气相色谱-质谱%农药残留%鳗鱼%三氯杀蟎醇
固相萃取%氣相色譜-質譜%農藥殘留%鰻魚%三氯殺蟎醇
고상췌취%기상색보-질보%농약잔류%만어%삼록살만순
Solid-Phase Extraction(SPE)%GC-MS%Pesticide Residues%Eels%Dicofol
建立了固相萃取-气相色谱串联质谱法检测鳗鱼中丁烯氟虫腈、三氯杀蟎醇等20种农药残留的分析方法。试样经乙腈提取后加入适量的去离子水和正己烷除去水溶性杂质和脂溶性杂质,再经填有中性氧化铝、C18和PSA混合填料的自组装固相萃取柱净化后进行GC-MS检测分析。采用选择离子扫描方式,用内标法进行定量。本方法简便、快速,方法的检出限(S/N=3)为0.001~0.009 mg/kg,在加标水平为0.01 mg/kg时,平均回收率为70.7~120%,相对标准偏差(RSD)为2.9~7.2%;在加标水平为0.02 mg/kg时,平均回收率为70.3~120%,相对标准偏差(RSD)为2.9~6.2%。
建立瞭固相萃取-氣相色譜串聯質譜法檢測鰻魚中丁烯氟蟲腈、三氯殺蟎醇等20種農藥殘留的分析方法。試樣經乙腈提取後加入適量的去離子水和正己烷除去水溶性雜質和脂溶性雜質,再經填有中性氧化鋁、C18和PSA混閤填料的自組裝固相萃取柱淨化後進行GC-MS檢測分析。採用選擇離子掃描方式,用內標法進行定量。本方法簡便、快速,方法的檢齣限(S/N=3)為0.001~0.009 mg/kg,在加標水平為0.01 mg/kg時,平均迴收率為70.7~120%,相對標準偏差(RSD)為2.9~7.2%;在加標水平為0.02 mg/kg時,平均迴收率為70.3~120%,相對標準偏差(RSD)為2.9~6.2%。
건립료고상췌취-기상색보천련질보법검측만어중정희불충정、삼록살만순등20충농약잔류적분석방법。시양경을정제취후가입괄량적거리자수화정기완제거수용성잡질화지용성잡질,재경전유중성양화려、C18화PSA혼합전료적자조장고상췌취주정화후진행GC-MS검측분석。채용선택리자소묘방식,용내표법진행정량。본방법간편、쾌속,방법적검출한(S/N=3)위0.001~0.009 mg/kg,재가표수평위0.01 mg/kg시,평균회수솔위70.7~120%,상대표준편차(RSD)위2.9~7.2%;재가표수평위0.02 mg/kg시,평균회수솔위70.3~120%,상대표준편차(RSD)위2.9~6.2%。
A method for the determination of multi pesticide multiresiduals such as flufiprole, dicofol in eels by gas chromatography with solid-phase extraction was proposed. The compounds were extracted from homogenized tissue with acetonitrile. Water-soluble and fat-soluble impurities in acetonitrile was removed by a moderate amount of hexane and deionized water. Acetonitrile extract purified by self-assembly solid-phase extraction column with mixed power of Alumina-N, C18 and PSA was ready for GC-MS analysis. The determination was performed in selected ion monitoring(SIM) mode with inner standard method for quantitative analysis. The detection limits(S/N=3)were in the range of 0.001~0.009 mg/kg.Tests for recovery were made by addition of mixed standards of 0.01 mg/kg,and the results were 70.7~120%,and the relative standard deviations were 2.9~7.2%. Tests for recovery were made by addition of mixed standards of 0.02 mg/kg,and the results were 70.3~120%,and the relative standard deviations were 2.9~6.2%.