China National Tobacco Quality Supervision and Test Center, Zhengzhou, P. R. China.
J Sep Sci. 2018 Nov;41(22):4233-4240. doi: 10.1002/jssc.201800861. Epub 2018 Oct 10.
For the purpose of chiral separation and determination of benalaxyl enantiomers in tobacco and soil, we developed a rapid, green, and sensitive method using ultra-performance convergence chromatography with tandem mass spectrometry. The samples were extracted and purified by the quick, easy, cheap, effective, rugged, and safe method before injection. The baseline separation was obtained on a chiral column in 5 min with carbon dioxide and ethanol as mobile phase. Separation parameters were optimized for the best separation efficiency. Under optimal conditions, the recoveries of both enantiomers were 77.1-98.4% with relative standard deviations <5.0% at spiked level of 0.1, 2.0, and 5.0 mg/kg in two matrices. Good coefficients of determination were achieved over the concentration range of 10-250 ng/mL. The limit of detection and the limit of quantification for all enantiomers ranged from 0.43 to 0.72 μg/kg and from 1.25 to 2.15 μg/kg, respectively. The results show that ultra-performance convergence chromatography with tandem mass spectrometry provides a reliable, green, and rapid method for the separation and determination of benalaxyl enantiomers in tobacco and soil. This method has important theoretical significance for studying the enantioselectivity and bioactivity of benalaxyl in the environment and in organisms.
为了在手性分离和测定烟草及土壤中西草净对映异构体方面的目的,我们开发了一种使用超高效相转化色谱-串联质谱法的快速、绿色和灵敏的方法。样品在进样前通过快速、简易、廉价、有效、耐用和安全的方法进行提取和纯化。在 5 分钟内,使用二氧化碳和乙醇作为流动相,在手性柱上实现了基线分离。通过优化分离参数,以获得最佳的分离效率。在最佳条件下,两种对映异构体在烟草和土壤中的回收率均为 77.1%-98.4%,相对标准偏差均<5.0%,在两个基质中的添加水平为 0.1、2.0 和 5.0mg/kg。在 10-250ng/mL 的浓度范围内,均获得了良好的线性关系。所有对映异构体的检出限和定量限范围分别为 0.43-0.72μg/kg 和 1.25-2.15μg/kg。结果表明,超高效相转化色谱-串联质谱法为分离和测定烟草及土壤中西草净对映异构体提供了一种可靠、绿色和快速的方法。该方法对于研究西草净在环境和生物体中的手性选择性和生物活性具有重要的理论意义。