色谱
色譜
색보
Chinese Journal of Chromatography
2015年
10期
1090-1096
,共7页
吴晓刚%陈孝权%肖海军%刘彬球
吳曉剛%陳孝權%肖海軍%劉彬毬
오효강%진효권%초해군%류빈구
超高效液相色谱-电喷雾串联质谱%柱前衍生化%草甘膦%草铵膦%茶
超高效液相色譜-電噴霧串聯質譜%柱前衍生化%草甘膦%草銨膦%茶
초고효액상색보-전분무천련질보%주전연생화%초감련%초안련%다
ultra high performance liquid chromatography-electrospray ionization tandem mass %spectrometry(UPLC-ESI-MS/MS)%pre-column derivatization%glyphosate(GLY)%glufosinate-ammonium( GLUF)%tea
采用超高效液相色谱-串联质谱建立了茶叶中草甘膦和草铵膦残留同时快速测定的方法。茶样经超纯水、二氯甲烷提取和C18固相萃取柱净化后，在硼酸盐缓冲液中与9-芴甲氧羰酰氯（ FMOC-Cl）进行衍生反应，衍生后产物在 C18色谱柱上进行超高效液相色谱分离；质谱检测采用电喷雾正离子化模式和多反应监测模式。结果表明，在0.003125~0.1 mg／L范围内，草甘膦和草铵膦均有良好的线性关系（ r>0.990），检出限（ LOD）均为0.03 mg／kg；在添加浓度为0.375、1.5和4.5 mg／kg时，草甘膦的平均回收率为87.37％~99.11％，相对标准偏差（ RSD）（ n=6）为0.68％~1.35％；草铵膦的平均回收率为81.44％~86.17％，RSD（ n=6）为1.01％~2.33％。该方法样品前处理简单，分析时间短，回收率和精密度等均符合农药多残留检测技术的要求，适用于茶叶中草甘膦和草铵膦残留的同时检测。
採用超高效液相色譜-串聯質譜建立瞭茶葉中草甘膦和草銨膦殘留同時快速測定的方法。茶樣經超純水、二氯甲烷提取和C18固相萃取柱淨化後，在硼痠鹽緩遲液中與9-芴甲氧羰酰氯（ FMOC-Cl）進行衍生反應，衍生後產物在 C18色譜柱上進行超高效液相色譜分離；質譜檢測採用電噴霧正離子化模式和多反應鑑測模式。結果錶明，在0.003125~0.1 mg／L範圍內，草甘膦和草銨膦均有良好的線性關繫（ r>0.990），檢齣限（ LOD）均為0.03 mg／kg；在添加濃度為0.375、1.5和4.5 mg／kg時，草甘膦的平均迴收率為87.37％~99.11％，相對標準偏差（ RSD）（ n=6）為0.68％~1.35％；草銨膦的平均迴收率為81.44％~86.17％，RSD（ n=6）為1.01％~2.33％。該方法樣品前處理簡單，分析時間短，迴收率和精密度等均符閤農藥多殘留檢測技術的要求，適用于茶葉中草甘膦和草銨膦殘留的同時檢測。
채용초고효액상색보-천련질보건립료다협중초감련화초안련잔류동시쾌속측정적방법。다양경초순수、이록갑완제취화C18고상췌취주정화후，재붕산염완충액중여9-물갑양탄선록（ FMOC-Cl）진행연생반응，연생후산물재 C18색보주상진행초고효액상색보분리；질보검측채용전분무정리자화모식화다반응감측모식。결과표명，재0.003125~0.1 mg／L범위내，초감련화초안련균유량호적선성관계（ r>0.990），검출한（ LOD）균위0.03 mg／kg；재첨가농도위0.375、1.5화4.5 mg／kg시，초감련적평균회수솔위87.37％~99.11％，상대표준편차（ RSD）（ n=6）위0.68％~1.35％；초안련적평균회수솔위81.44％~86.17％，RSD（ n=6）위1.01％~2.33％。해방법양품전처리간단，분석시간단，회수솔화정밀도등균부합농약다잔류검측기술적요구，괄용우다협중초감련화초안련잔류적동시검측。
A method was developed for the determination of glyphosate( GLY)and glufosinate-ammonium( GLUF)in tea using ultra performance liquid chromatography-tandem mass spec-trometry( UPLC-MS/MS). The sample was extracted with ultrapure water and dichloromethane for 30 min under ultrasonication,followed by a simple cleanup with a C 18 solid phase extraction ( SPE)cartridge,and then GLY and GLUF were derivatized using 9-fluorenylmethoxycarbonyl (FMOC-Cl)in borate buffer for 2 h. The derivatives of GLY and GLUF were separated on a Waters C18 column(50 mm×2. 1 mm,1. 7 μm)in a gradient elution mode,and finally detected with positive electrospray ionization-mass spectrometry ( ESI-MS/MS ) in multiple reaction monitoring( MRM ) mode. The quantification analysis was performed by external standard method. The method showed a good linearity( r>0. 990)in the range of 0. 003 125-0. 1 mg/L. The limits of detection( LODs)of GLY and GLUF were 0. 03 mg/kg. At the spiked levels of 0. 375,1. 5 and 4. 5 mg/kg,the recoveries of GLY and GLUF were 87. 37%-99. 11% and 81. 44%-86. 17% respectively,and the relative standard deviations( RSDs)( n=6)of GLY and GLUF were 0. 68%-1. 35% and 1. 01%-2. 33%,respectively. This method is simple,rapid and charac-terized with acceptable sensitivity and accuracy to meet the requirements for the analysis of GLY and GLUF simultaneously in tea.
