农药学学报
農藥學學報
농약학학보
CHINESE JOURNAL OF PESTICIDE SCIENCE
2014年
5期
614-618
,共5页
张月%林靖凌%韩丙军%吕岱竹
張月%林靖凌%韓丙軍%呂岱竹
장월%림정릉%한병군%려대죽
超高效液相色谱-三重四级杆串联质谱%柑橘%苯甲酰脲类农药%残留
超高效液相色譜-三重四級桿串聯質譜%柑橘%苯甲酰脲類農藥%殘留
초고효액상색보-삼중사급간천련질보%감귤%분갑선뇨류농약%잔류
ultra performance liquid chromatography-tandem mass spectrometry ( UPLC-MS/MS )%citrus fruit%benzoylurea pesticides%residue
建立了柑橘中虱螨脲、灭幼脲、氟啶脲和除虫脲4种苯甲酰脲类农药同时检测的超高效液相色谱-三重四级杆串联质谱( UPLC-MS/MS)分析方法。样品采用QuEChERS前处理技术,超高效液相色谱-串联质谱电喷雾负离子模式检测测定。结果表明:在0.01~0.2μg/mL范围内,4种供试农药的质量浓度与其相应的峰面积间呈良好的线性关系,相关系数( r )均大于0.994。在0.01、0.05和0.1 mg/kg 3个添加水平下,4种农药的平均回收率为92%~105%,相对标准偏差(RSD)为0.4%~3.3%(n=5)。4种农药在柑橘中的定量限(LOQ)均为0.01 mg/kg。该方法准确、灵敏、简单,适用于同时测定柑橘中4种苯甲酰脲类农药的残留量。
建立瞭柑橘中虱螨脲、滅幼脲、氟啶脲和除蟲脲4種苯甲酰脲類農藥同時檢測的超高效液相色譜-三重四級桿串聯質譜( UPLC-MS/MS)分析方法。樣品採用QuEChERS前處理技術,超高效液相色譜-串聯質譜電噴霧負離子模式檢測測定。結果錶明:在0.01~0.2μg/mL範圍內,4種供試農藥的質量濃度與其相應的峰麵積間呈良好的線性關繫,相關繫數( r )均大于0.994。在0.01、0.05和0.1 mg/kg 3箇添加水平下,4種農藥的平均迴收率為92%~105%,相對標準偏差(RSD)為0.4%~3.3%(n=5)。4種農藥在柑橘中的定量限(LOQ)均為0.01 mg/kg。該方法準確、靈敏、簡單,適用于同時測定柑橘中4種苯甲酰脲類農藥的殘留量。
건립료감귤중슬만뇨、멸유뇨、불정뇨화제충뇨4충분갑선뇨류농약동시검측적초고효액상색보-삼중사급간천련질보( UPLC-MS/MS)분석방법。양품채용QuEChERS전처리기술,초고효액상색보-천련질보전분무부리자모식검측측정。결과표명:재0.01~0.2μg/mL범위내,4충공시농약적질량농도여기상응적봉면적간정량호적선성관계,상관계수( r )균대우0.994。재0.01、0.05화0.1 mg/kg 3개첨가수평하,4충농약적평균회수솔위92%~105%,상대표준편차(RSD)위0.4%~3.3%(n=5)。4충농약재감귤중적정량한(LOQ)균위0.01 mg/kg。해방법준학、령민、간단,괄용우동시측정감귤중4충분갑선뇨류농약적잔류량。
A ultra performance liquid chromatography-tandem mass spectrometry ( UPLC-MS/MS ) method for the simultaneous determination of 4 benzoylurea pesticides ( lufenuron, chlorbenzuron, chlorfluazuron and diflubenzuron ) in citrus fruits was established. The procedure was based on QuEChERS cleanup and determination with UPLC-MS/MS. The results showed that the calibration curve was linear in the range of 0. 01-0. 2 mg/mL and correlation coefficient(r) higher than 0. 994. The average recoveries of 4 pesticides were 92% -105% when the spiked levels were 0. 01 , 0. 05 and 0. 1 mg/kg, with relative standard deviations (RSD) between 0. 4% and 3. 3% (n=5). The limits of quantitation ( LOQ) for 4 pesticides were 0. 01 mg/kg. The method is accurate, sensitive, simple, suitable for the simultaneous determination of 4 pesticide residues in citrus fruits.