Chen Junhui, Liu Jie, Lee Frank Sen-Chun, Wang Xiaoru
College of Chemistry and Chemical Engineering, Ocean University of China, Qingdao, China.
J Sep Sci. 2008 Jan;31(1):137-42. doi: 10.1002/jssc.200700239.
HPLC coupled online with atmospheric pressure chemical ionization MS (APCI-MS) technique was evaluated for the qualitative and quantitative determination of solanesol in extracts of tobacco leaves. The solanesol and other compounds in the extract were separated on an Alltima C(8) (4.6 mm x 250 mm) column with methanol and water (98:2 v/v) as mobile phase, with flow rate of 0.8 mL/min and UV detection wavelength of 211 nm. In the APCI(+) mode, abundant stable M-H(2)O + H ion (m/z at 613.5) was observed, with low abundance of other fragmentation ions. A comparison of APCI-MS and ESI-MS techniques showed that APCI mode is more sensitive than ESI mode, and thus better suited for solanesol analysis. When comparing UV 211 nm and APCI-MS in SIM for solanesol quantification, the former offered better precision and reproducibility, but the latter was more than 200 times sensitive in detection. The developed method has been successfully applied to the analysis and comparison of solanesol concentration in different tobacco leaf samples.
采用高效液相色谱(HPLC)与大气压化学电离质谱(APCI-MS)联用技术对烟草叶提取物中的茄尼醇进行定性和定量测定。提取物中的茄尼醇和其他化合物在Alltima C(8)(4.6 mm×250 mm)色谱柱上分离,以甲醇和水(98:2 v/v)为流动相,流速为0.8 mL/min,紫外检测波长为211 nm。在APCI(+)模式下,观察到丰富稳定的M-H₂O + H离子(m/z为613.5),其他碎片离子丰度较低。APCI-MS和ESI-MS技术的比较表明,APCI模式比ESI模式更灵敏,因此更适合茄尼醇分析。在对茄尼醇进行定量分析时,比较紫外211 nm和APCI-MS的选择离子监测(SIM)模式,前者具有更好的精密度和重现性,但后者的检测灵敏度高出200多倍。所建立的方法已成功应用于不同烟草叶样品中茄尼醇浓度的分析和比较。