Li Yuanbo, Dong Fengshou, Liu Xingang, Xu Jun, Li Jing, Kong Zhiqiang, Chen Xiu, Zheng Yongquan
Institute of Plant Protection, Chinese Academy of Agricultural Sciences, Key Laboratory of Pesticide Chemistry and Application, Ministry of Agriculture, Beijing, P. R. China.
J Sep Sci. 2012 Jan;35(2):206-15. doi: 10.1002/jssc.201100674. Epub 2011 Dec 12.
A novel and sensitive method was developed for the determination of tebuconazole enantioselectively using reversed-phase LC-MS/MS. The separation and determination were performed using on an amylose-based chiral stationary phase, a Lux 3u Amylose-2 column (150 mm×2.0 mm), under isocratic conditions at 0.3 mL/min flow rate. A series of chiral stationary phases were investigated and the effect of mobile phase composition on the enantioseparation was discussed. Parameters including the matrix effect, linearity, precision, accuracy and stability were evaluated. Under optimal conditions, the overall mean recoveries for two enantiomers from the soil, tomato, cucumber, pear and apple samples were 79.3-101.1% with 2.8-11.5% intra-day relative standard deviations (RSDs) and 4.1-8.6% inter-day RSDs at 5, 25 and 50 μg/kg levels; the mean enantiomer recoveries from the water samples were 89.6-101.9% with 3.3-10.2% intra-day RSDs and 5.1-7.7% inter-day RSDs at 0.25, 0.5 and 2.5 μg/kg levels. The limits of detection (LODs) for all enantiomers in tomato, cucumber, pear, apple, soil and water were less than 0.6 μg/kg, whereas the limit of quantification (LOQ) did not exceed 2.0 μg/kg. The results indicate that this proposed method is convenient and reliable for the enantioselective determination of tebuconazole enantiomers in foods and environment samples.
建立了一种新颖且灵敏的方法,用于使用反相液相色谱-串联质谱法对戊唑醇进行对映体选择性测定。分离和测定在直链淀粉基手性固定相(Lux 3u Amylose-2柱,150 mm×2.0 mm)上进行,在等度条件下,流速为0.3 mL/min。研究了一系列手性固定相,并讨论了流动相组成对映体分离的影响。评估了包括基质效应、线性、精密度、准确度和稳定性在内的参数。在最佳条件下,在5、25和50 μg/kg水平下,从土壤、番茄、黄瓜、梨和苹果样品中两种对映体的总体平均回收率为79.3-101.1%,日内相对标准偏差(RSD)为2.8-11.5%,日间RSD为4.1-8.6%;在0.25、0.5和2.5 μg/kg水平下,水样中对映体的平均回收率为89.6-101.9%,日内RSD为3.3-10.2%,日间RSD为5.1-7.7%。番茄、黄瓜、梨、苹果、土壤和水中所有对映体的检测限(LOD)均小于0.6 μg/kg,而定量限(LOQ)不超过2.0 μg/kg。结果表明,该方法对于食品和环境样品中戊唑醇对映体的对映体选择性测定方便且可靠。