分析仪器
分析儀器
분석의기
ANALYTICAL INSTRUMENTATION
2014年
2期
47-51
,共5页
孙涛%刘圣红%赵子刚%古丽斯坦%赵多勇%王成
孫濤%劉聖紅%趙子剛%古麗斯坦%趙多勇%王成
손도%류골홍%조자강%고려사탄%조다용%왕성
超高效液相色谱-串联质谱%食用菌%多残留
超高效液相色譜-串聯質譜%食用菌%多殘留
초고효액상색보-천련질보%식용균%다잔류
Ultra performance liquid chromatography-tandem mass spectrometry%edible fungus%multi-residues
采用超高效液相色谱-串联质谱(U PLC -M S/M S )技术,建立了同时检测食用菌中10种农药的多残留检测方法。样品经乙腈提取,氨基固相萃取柱净化,Waters HSST3超高效液相色谱柱分离,进入电喷雾串联四极杆质谱进行检测,采用多反应监测(M RM )分析,对液质分离条件和样品前处理条件进行了优化。结果表明10种农药在10~200μg/L 范围内线性良好(r≥0.9985)。在0.01、0.05 mg/kg 浓度范围内,平均加标回收率在80.3%~102.6%之间;相对标准偏差RSD (%)≤9.8%。该方法的最低检出限范围为1.72×10-4~9.28×10-3 mg/kg。该方法简便、快速、灵敏、净化效果好,测定结果满足食用菌农药多残留的检测要求。
採用超高效液相色譜-串聯質譜(U PLC -M S/M S )技術,建立瞭同時檢測食用菌中10種農藥的多殘留檢測方法。樣品經乙腈提取,氨基固相萃取柱淨化,Waters HSST3超高效液相色譜柱分離,進入電噴霧串聯四極桿質譜進行檢測,採用多反應鑑測(M RM )分析,對液質分離條件和樣品前處理條件進行瞭優化。結果錶明10種農藥在10~200μg/L 範圍內線性良好(r≥0.9985)。在0.01、0.05 mg/kg 濃度範圍內,平均加標迴收率在80.3%~102.6%之間;相對標準偏差RSD (%)≤9.8%。該方法的最低檢齣限範圍為1.72×10-4~9.28×10-3 mg/kg。該方法簡便、快速、靈敏、淨化效果好,測定結果滿足食用菌農藥多殘留的檢測要求。
채용초고효액상색보-천련질보(U PLC -M S/M S )기술,건립료동시검측식용균중10충농약적다잔류검측방법。양품경을정제취,안기고상췌취주정화,Waters HSST3초고효액상색보주분리,진입전분무천련사겁간질보진행검측,채용다반응감측(M RM )분석,대액질분리조건화양품전처리조건진행료우화。결과표명10충농약재10~200μg/L 범위내선성량호(r≥0.9985)。재0.01、0.05 mg/kg 농도범위내,평균가표회수솔재80.3%~102.6%지간;상대표준편차RSD (%)≤9.8%。해방법적최저검출한범위위1.72×10-4~9.28×10-3 mg/kg。해방법간편、쾌속、령민、정화효과호,측정결과만족식용균농약다잔류적검측요구。
An ultra performance liquid chromatography-tandem mass spectrometric method (UPLC-MS/MS) is developed for the simultaneous determination of 10 residues in edible fungus .The pesticides were extracted with acetonitrile ,cleaned up with NH2 solid phase extraction cartridge (SPE) .The UPLC analysis are performed on an Acuity UPLC HSST3column with gradient eluation ,combining with multiple reaction monitoring (MRM ) mode .The linear range is 10-200μg/L ,the correlation coefficients is above 0.9985 in the linear range .The average recoveries of 10 pesticides in spiked fungus (0 .01 and 0 .05mg/kg) is 80 .3%-102 .6% ,and the relative standard deviation is below 9 .8% .T he results indicate that the meth-od is easier ,faster ,more sensitive and better purification effect .And the method can meet the require-ments for simultaneous determination of multi-residues in edible fungus .