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Analytical method validation for terbutryn using gas chromatography/ion trap gas chromatography/mass selective detector and liquid chromatography/triple quadrupole mass spectrometers

机译:使用气相色谱/离子阱气相色谱/质量选择检测器和液相色谱/三重四极杆质谱仪对叔丁草进行分析方法验证

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摘要

Analytical methods including solvent extraction followed by gas chromatography/ion-trap (GC/IT) with scan and MS/MS mode, a GC/mass selective detector (GC/MSD), and liquid chromatography/triple quadrupole mass spectrometers (LC/MS/MS) were optimized to identify and quantify terbutryn. The spike recovery was 96.5% using GC/IT with scan mode and 103.5% with MS/MS mode, 90.3% by GC/MSD, and 92.5% by LC/MS/MS. The limit of detection (LOD) was 0.0015 mg/kg by GC/IT with scan, 0.026 mg/kg with MS/MS mode, 0.015 mg/kg with GC/MSD, and 0.026 mg/kg by LC/MS/MS. Of the four methods, GC/IT with scan mode was determined to be the most sensitive (with LOD: 0.0015 mg/kg and limit of quantitation (LOQ): 0.0047 mg/kg), rapid (retention time: 9.6 min) and the most precise method (relative standard deviation: 17%) for the quantification of terbutryn. GC/IT with scan mode proved to be the more sensitive analytical method for terbutryn than other methods in this study, showing better accuracy and rapid analysis.
机译:分析方法包括溶剂萃取,然后是带有扫描和MS / MS模式的气相色谱/离子阱(GC / IT),GC /质谱选择性检测器(GC / MSD)和液相色谱/三重四极杆质谱仪(LC / MS) / MS)进行了优化,以鉴定和定量特布丁。使用GC / IT扫描模式时,加标回收率为96.5%;使用MS / MS模式时,为103.5%;通过GC / MSD检测时,为90.3%;通过LC / MS / MS检测时,为92.5%。 GC / IT扫描的检出限(LOD)为0.0015 mg / kg,MS / MS模式的检出限为0.026 mg / kg,GC / MSD的检出限为0.015 mg / kg,LC / MS / MS的检出限为0.026 mg / kg。在这四种方法中,采用扫描模式的GC / IT被确定为最敏感的(LOD:0.0015 mg / kg,定量限(LOQ):0.0047 mg / kg),快速(保留时间:9.6 min)和最精确的方法(相对标准偏差:17%)用于叔丁精的定量。在本研究中,采用扫描模式的GC / IT被证明是特丁菌灵的更灵敏的分析方法,显示了更高的准确性和快速的分析。

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