湖南林业科技
湖南林業科技
호남임업과기
Hunan Forestry Science & Technology
2015年
5期
46-49
,共4页
李玉平%佘佳荣%谭利娟%邓红波
李玉平%佘佳榮%譚利娟%鄧紅波
리옥평%사가영%담리연%산홍파
油茶籽%液相色谱-串联质谱法%农药残留
油茶籽%液相色譜-串聯質譜法%農藥殘留
유다자%액상색보-천련질보법%농약잔류
camellia seed%liquid chromatography with tandem mass spectrometry%residue
建立了高效液相色谱串联-质谱法同时检测油茶籽中吡虫啉、乐果、甲胺磷、马拉硫磷、三唑酮、对硫磷、毒死蜱、丁草胺、噻嗪酮9种农药的残留量。样品经乙腈提取后,取上清液直接过膜后进行液相色谱串联质谱分析。采用 Agilent SB—C18色谱柱分离,用4 g/L 甲酸铵水溶液-乙腈作为流动相进行梯度洗脱,电喷雾正离子(ESI +)模式电离,多反应监测(MRM)模式检测。结果表明:各物质峰面积与样品浓度在0.001~0.5 mg/L 范围内呈良好的线性关系,线性回归系数大于0.9990。在添加浓度0.01~1.0 mg/kg 范围内,9种农药的平均添加回收率在64.2%~114.1%范围内,变异系数在1.2%~9.4%之间,该方法能满足油茶籽中9种农药残留量分析的要求。
建立瞭高效液相色譜串聯-質譜法同時檢測油茶籽中吡蟲啉、樂果、甲胺燐、馬拉硫燐、三唑酮、對硫燐、毒死蜱、丁草胺、噻嗪酮9種農藥的殘留量。樣品經乙腈提取後,取上清液直接過膜後進行液相色譜串聯質譜分析。採用 Agilent SB—C18色譜柱分離,用4 g/L 甲痠銨水溶液-乙腈作為流動相進行梯度洗脫,電噴霧正離子(ESI +)模式電離,多反應鑑測(MRM)模式檢測。結果錶明:各物質峰麵積與樣品濃度在0.001~0.5 mg/L 範圍內呈良好的線性關繫,線性迴歸繫數大于0.9990。在添加濃度0.01~1.0 mg/kg 範圍內,9種農藥的平均添加迴收率在64.2%~114.1%範圍內,變異繫數在1.2%~9.4%之間,該方法能滿足油茶籽中9種農藥殘留量分析的要求。
건립료고효액상색보천련-질보법동시검측유다자중필충람、악과、갑알린、마랍류린、삼서동、대류린、독사비、정초알、새진동9충농약적잔류량。양품경을정제취후,취상청액직접과막후진행액상색보천련질보분석。채용 Agilent SB—C18색보주분리,용4 g/L 갑산안수용액-을정작위류동상진행제도세탈,전분무정리자(ESI +)모식전리,다반응감측(MRM)모식검측。결과표명:각물질봉면적여양품농도재0.001~0.5 mg/L 범위내정량호적선성관계,선성회귀계수대우0.9990。재첨가농도0.01~1.0 mg/kg 범위내,9충농약적평균첨가회수솔재64.2%~114.1%범위내,변이계수재1.2%~9.4%지간,해방법능만족유다자중9충농약잔류량분석적요구。
A method was developed for determining 9 pesticides residues in camellia seed using liquid chromatography tandem mass spectrometry.Samples were extracted with acetonitrile.Then,the upper supernatant was directly analyzed by LC —MS /MS on an Agilent SB—C18 column with a mixture of 4g/L formic acid ammonium solution (A)and acetoni-trile (B)as mobile phase under gradient elution conditions.The mass spectrometer operated in multiple reaction monito-ring (MRM)mode with the positive mode.There is a good linear correlation (all of the calibration coefficients are above 0.9990)between the peak areas and concentration of sixteen amide fungicides in the range of 0.001 ~0.5 mg/L.The average recoveries of 9 pesticides in camellia seed were 64.2% ~114.1%.The relative standard deviations were between 1.2% and 9.4%.The method is demonstrated to be suitable for the determination of the 9 kinds of pesticides in camellia seed.