Li J S, Chen M, Li Z C
Intertek-AAC Labs, 711 Parkland Court, Champaign, Illinois, 61821.
Anal Chem Insights. 2012;7:47-58. doi: 10.4137/ACI.S9969. Epub 2012 Aug 6.
A sensitive and reliable method of liquid chromatography-electrospray ionization/tandem mass spectrometry (LC-ESI/MS/ MS) was developed and validated for determining 1,3-dimethylamylamine (1,3-DMAA) and 1,4-dimethylamylamine (1,4-DMAA) in geranium plants (Pelargonium graveolens). The sample was extracted with 0.5 M HCl and purified by liquid-liquid partition with hexane. The parameters for reverse-phase (C18) LC and positive ESI/MS/MS were optimized. The matrix effect, specificity, linearity, precision, accuracy and reproducibility of the method were determined and evaluated. The method was linear over a range of 0.10-10.00 ng/mL examined, with R(2) of 0.99 for both 1,3-DMAA and 1,4-DMAA. The recoveries from spiked concentrations between 5.00-40.00 ng/g were 85.1%-104.9% for 1,3-DMAA, with relative standard deviation (RSD) of 2.9%-11.0%, and 82.9%-101.8% for 1,4-DMAA, with RSD of 3.2%-11.7%. The instrument detection limit was 1-2 pg for both DMAAs. The quantification limit was estimated to be 1-2 ng/g for the plant sample. This method was successfully applied to the quantitative determination of 1,3- and 1,4-DMAA in both geranium plant and geranium oil.
建立了一种灵敏可靠的液相色谱 - 电喷雾电离/串联质谱法(LC - ESI/MS/MS),并对天竺葵(Pelargonium graveolens)植株中1,3 - 二甲基戊胺(1,3 - DMAA)和1,4 - 二甲基戊胺(1,4 - DMAA)的含量测定方法进行了验证。样品用0.5 M盐酸萃取,并用己烷液 - 液分配法纯化。对反相(C18)液相色谱和正离子电喷雾电离串联质谱的参数进行了优化。测定并评估了该方法的基质效应、特异性、线性、精密度、准确度和重现性。在所检测的0.10 - 10.00 ng/mL范围内,该方法呈线性,1,3 - DMAA和1,4 - DMAA的R²均为0.99。加标浓度在5.00 - 40.00 ng/g之间时,1,3 - DMAA的回收率为85.1% - 104.9%,相对标准偏差(RSD)为2.9% - 11.0%;1,4 - DMAA的回收率为82.9% - 101.8%,RSD为3.2% - 11.7%。两种二甲基戊胺的仪器检测限均为1 - 2 pg。植物样品的定量限估计为1 - 2 ng/g。该方法成功应用于天竺葵植株和天竺葵油中1,3 - 和1,4 - DMAA的定量测定。