食品研究与开发
食品研究與開髮
식품연구여개발
FOOD RESEARCH AND CEVELOPMENT
2015年
3期
100-103
,共4页
晏利芝%赵永彪%刘宁%宋薇
晏利芝%趙永彪%劉寧%宋薇
안리지%조영표%류저%송미
多残留检测%QuEChERS农残净化管%蔬菜%超高液相色谱-串联质谱
多殘留檢測%QuEChERS農殘淨化管%蔬菜%超高液相色譜-串聯質譜
다잔류검측%QuEChERS농잔정화관%소채%초고액상색보-천련질보
Mult-i residue analysis%solid phase extraction%vegetables%ultra performance liquid chromatogra-phy-tandem mass spectrometry
采用超高液相色谱-串联质谱联用仪(UPLC-MS/MS)技术建立了同时检测蔬菜中34种农药多残留量的快速检测方法。样品经乙腈提取,浓缩定容后用QuEChERS农残净化管净化,Acquity BEH-C18超高液相色谱柱分离,进入电喷雾串联四极杆质谱进行检测,采用多反应监测(MRM)分析,对液质分离条件进行优化。结果表明34种农药在10 ng/mL~200 ng/mL范围内线性良好(r≥0.9936)。在10μg/kg~30μg/kg范围内,平均加标回收率在68.7%~116.8%之间,RSD≤12%。该方法检出限为0.001 mg/kg~0.01 mg/kg,测定结果满足蔬菜样品中多残留农药的检测要求。
採用超高液相色譜-串聯質譜聯用儀(UPLC-MS/MS)技術建立瞭同時檢測蔬菜中34種農藥多殘留量的快速檢測方法。樣品經乙腈提取,濃縮定容後用QuEChERS農殘淨化管淨化,Acquity BEH-C18超高液相色譜柱分離,進入電噴霧串聯四極桿質譜進行檢測,採用多反應鑑測(MRM)分析,對液質分離條件進行優化。結果錶明34種農藥在10 ng/mL~200 ng/mL範圍內線性良好(r≥0.9936)。在10μg/kg~30μg/kg範圍內,平均加標迴收率在68.7%~116.8%之間,RSD≤12%。該方法檢齣限為0.001 mg/kg~0.01 mg/kg,測定結果滿足蔬菜樣品中多殘留農藥的檢測要求。
채용초고액상색보-천련질보련용의(UPLC-MS/MS)기술건립료동시검측소채중34충농약다잔류량적쾌속검측방법。양품경을정제취,농축정용후용QuEChERS농잔정화관정화,Acquity BEH-C18초고액상색보주분리,진입전분무천련사겁간질보진행검측,채용다반응감측(MRM)분석,대액질분리조건진행우화。결과표명34충농약재10 ng/mL~200 ng/mL범위내선성량호(r≥0.9936)。재10μg/kg~30μg/kg범위내,평균가표회수솔재68.7%~116.8%지간,RSD≤12%。해방법검출한위0.001 mg/kg~0.01 mg/kg,측정결과만족소채양품중다잔류농약적검측요구。
An ultra performance liquid chromatography-tandem mass spectrometric method (UPLC-MS/MS) has been developed for the simultaneous determination of 34 kinds of pesticide residues and the metabolites in vegetables. The samples were extracted by acetonitrile and purificated with QuE ChERS.The UPLC analyses were performed on an acquity UPLC C18 column with gradient eluation , combined withionization in positive mode ( ESI+) and multiple react ion monitoring (MRM) mode. The linear range was 10 ng/mL-200 ng/mL, and the correlation coefficients were more than 0.993 6. The average recoveries of 34 kinds of pesticidesin spiked vegetables (10 and 30μg/kg) ranged from 68.7 %to 116.8 %and the relative standard deviation were not more than 12 %.The detection limits were 0.001 mg/kg-0.01 mg/kg .The mult-i residue analysis method can meet the requirements for imultaneous determinationof mult-i pesticides residues in vegetables.