山东化工
山東化工
산동화공
SHANDONG CHEMICAL INDUSTRY
2014年
7期
70-72
,共3页
液相色谱 - 串联质谱%草甘膦%衍生反应
液相色譜 - 串聯質譜%草甘膦%衍生反應
액상색보 - 천련질보%초감련%연생반응
HPLC - tandem mass spectrometry%glyphosate%derivative reaction
采用高效液相色谱串联质谱建立了武夷岩茶样品中草甘膦的残留量的测定方法。样品经水固相萃取和茶叶专用萃取柱（TPT）净化后，在硼酸盐缓冲液中与9-芴甲基氯甲酸酯（FMOC - Cl）进行衍生化反应，以1％乙酸铵溶液和乙腈为流动相，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，草甘膦在1~10 ng/ mL 范围内线性良好，线性相关系数 r =0.998。通过对空白武夷岩茶样品进行4个加标水平的添加回收实验（n =5），草甘膦的平均回收率和相对标准偏差（RSD）分别为87.3％~98.0％和3.46~5.12。
採用高效液相色譜串聯質譜建立瞭武夷巖茶樣品中草甘膦的殘留量的測定方法。樣品經水固相萃取和茶葉專用萃取柱（TPT）淨化後，在硼痠鹽緩遲液中與9-芴甲基氯甲痠酯（FMOC - Cl）進行衍生化反應，以1％乙痠銨溶液和乙腈為流動相，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，草甘膦在1~10 ng/ mL 範圍內線性良好，線性相關繫數 r =0.998。通過對空白武夷巖茶樣品進行4箇加標水平的添加迴收實驗（n =5），草甘膦的平均迴收率和相對標準偏差（RSD）分彆為87.3％~98.0％和3.46~5.12。
채용고효액상색보천련질보건립료무이암다양품중초감련적잔류량적측정방법。양품경수고상췌취화다협전용췌취주（TPT）정화후，재붕산염완충액중여9-물갑기록갑산지（FMOC - Cl）진행연생화반응，이1％을산안용액화을정위류동상，질보검측채용전분무정리자화모식화다반응감측모식。결과표명，초감련재1~10 ng/ mL 범위내선성량호，선성상관계수 r =0.998。통과대공백무이암다양품진행4개가표수평적첨가회수실험（n =5），초감련적평균회수솔화상대표준편차（RSD）분별위87.3％~98.0％화3.46~5.12。
A method for determination of glyphosate residues in Wuyi rock tea was developed using high performance liquid chromatography tandem mass spectrometry method. The procedure is as follow,the glyphosate were extracted with water from samples, and purified using TPT. Then derivatization reaction was done in borate buffer with fluorenylmethylchloroformate(FMOC - Cl). Using 1% solution of ammonium acetate and acetonitrile as the mobile phase, mass spectrometry using electrospray ionization in positive ionization mode and multiple reaction monitoring mode. The results showed that the linear correlation coefficient r = 0. 998 when glyphosate is between1ng - 10ng/ mL. Wuyi blank samples were used in added recovery experiment at four spiked levels(n = 5),the average recovery of glyphosate were 87. 3% to 98. 0% . The relative standard deviation(RSD)were 3. 46 to 5. 12.
