色谱
色譜
색보
Chinese Journal of Chromatography
2015年
10期
1019-1025
,共7页
马琳%陈建波%赵莉%占绣萍
馬琳%陳建波%趙莉%佔繡萍
마림%진건파%조리%점수평
超高效液相色谱-串联质谱%固相萃取%酰胺类农药%残留%蔬菜%水果
超高效液相色譜-串聯質譜%固相萃取%酰胺類農藥%殘留%蔬菜%水果
초고효액상색보-천련질보%고상췌취%선알류농약%잔류%소채%수과
ultra high performance liquid chromatography-tandem mass spectrometry( UPLC-MS/MS)%solid phase extraction( SPE)%amide pesticides%residues%vegetables%fruits
建立了同时测定果蔬中6种酰胺类农药的固相萃取-超高效液相色谱-串联质谱（ SPE-UPLC-MS／MS）方法。样品经乙腈高速匀浆提取、Florisil固相萃取柱净化，采用超高效液相色谱-串联质谱法测定6种农药。质谱分析采用电喷雾电离，正负双离子扫描，多反应监测（ MRM）模式。结果表明：6种农药在0.0005~1.00 mg／L范围内均呈现良好的线性关系，相关系数均大于0.999；在0.01、0.1和1.0 mg／kg（氟苯虫酰胺为0.001、0.01和0.1 mg／kg）3个浓度添加水平下的平均回收率为72.4％~119.4％，相对标准偏差（ n=5）小于15％；定量限为0.01 mg／kg（溴氰虫酰胺、双炔酰菌胺、啶酰菌胺、氟吡菌胺和噻呋酰胺）和0.001 mg／kg（氟苯虫酰胺）。该方法简单、快速、重现性好、灵敏度高，可满足果蔬中6种酰胺类农药残留检测的要求。
建立瞭同時測定果蔬中6種酰胺類農藥的固相萃取-超高效液相色譜-串聯質譜（ SPE-UPLC-MS／MS）方法。樣品經乙腈高速勻漿提取、Florisil固相萃取柱淨化，採用超高效液相色譜-串聯質譜法測定6種農藥。質譜分析採用電噴霧電離，正負雙離子掃描，多反應鑑測（ MRM）模式。結果錶明：6種農藥在0.0005~1.00 mg／L範圍內均呈現良好的線性關繫，相關繫數均大于0.999；在0.01、0.1和1.0 mg／kg（氟苯蟲酰胺為0.001、0.01和0.1 mg／kg）3箇濃度添加水平下的平均迴收率為72.4％~119.4％，相對標準偏差（ n=5）小于15％；定量限為0.01 mg／kg（溴氰蟲酰胺、雙炔酰菌胺、啶酰菌胺、氟吡菌胺和噻呋酰胺）和0.001 mg／kg（氟苯蟲酰胺）。該方法簡單、快速、重現性好、靈敏度高，可滿足果蔬中6種酰胺類農藥殘留檢測的要求。
건립료동시측정과소중6충선알류농약적고상췌취-초고효액상색보-천련질보（ SPE-UPLC-MS／MS）방법。양품경을정고속균장제취、Florisil고상췌취주정화，채용초고효액상색보-천련질보법측정6충농약。질보분석채용전분무전리，정부쌍리자소묘，다반응감측（ MRM）모식。결과표명：6충농약재0.0005~1.00 mg／L범위내균정현량호적선성관계，상관계수균대우0.999；재0.01、0.1화1.0 mg／kg（불분충선알위0.001、0.01화0.1 mg／kg）3개농도첨가수평하적평균회수솔위72.4％~119.4％，상대표준편차（ n=5）소우15％；정량한위0.01 mg／kg（추청충선알、쌍결선균알、정선균알、불필균알화새부선알）화0.001 mg／kg（불분충선알）。해방법간단、쾌속、중현성호、령민도고，가만족과소중6충선알류농약잔류검측적요구。
A solid phase extraction coupled with ultra high performance liquid chromatography-tandem mass spectrometry ( SPE-UPLC-MS/MS ) method was developed for simultaneous determination of six amide pesticides,cyantraniliprole,mandipropamid,boscalid,fluopicol-ide,thifluzamide and flubendiamide,in vegetables and fruits. After extraction with acetonitrile, purification with Florisil SPE cartridges and dissolution with methanol,the targets in the sam-ple solutions were analyzed by UPLC-MS/MS on an Agilent Proshell 120 EC-C18 column with a mixture of 0. 1% formic acid solution and methanol as the mobile phases under gradient elution conditions. The mass spectrometer operated in multiple reaction monitoring( MRM)mode with the negative and positive modes. Good linearity was obtained for the six amide pesticides at the mass concentrations of 0. 000 5-1. 00mg/L with the correlation coefficients more than 0. 999. The fortified recoveries were in the range of 72. 4%-119. 4% with the concentration levels at 0. 01,0. 1 and 1. 0 mg/kg for cyantraniliprole,mandipropamid,boscalid,fluopicolide,thi-fluzamide,and 0. 001,0. 01 and 0. 1 mg/kg for flubendiamide. The relative standard deviations ( RSDs)were less than 15% and the limits of quantification were 0. 01 mg/kg for cyantranilipro-le,mandipropamid,boscalid,fluopicolide,thifluzamide,and 0. 001 mg/kg for flubendiamide. All the above observations indicate that the established analytical method is simple ,efficient and sensitive,and suitable for the determination of the six amide pesticides in vegetables and fruits.
