Department of Pharmacy, Peking University, Beijing 100191, China.
J Chromatogr A. 2010 Dec 24;1217(52):8317-26. doi: 10.1016/j.chroma.2010.10.093. Epub 2010 Oct 30.
The applicability of comprehensive two-dimensional gas chromatography (GC×GC) for flavonoids analysis was investigated by separation and identification of flavonoids in standards, and a complex matrix natural sample. The modulation temperature was optimized to achieve the best separation and signal enhancement. The separation pattern of trimethylsilyl (TMS) derivatives of flavonoids was compared on two complementary column sets. Whilst the BPX5/BPX50 (NP/P) column set offers better overall separation, BPX50/BPX5 (P/NP) provides better peak shape and sensitivity. Comparison of the identification power of GC×GC-TOFMS against both the NIST05 MS library and a laboratory (created in-house) TOFMS library was carried out on a flavonoid mixture. The basic retention index information on high-performance capillary columns with a non-polar stationary phase was established and database of mass spectra of trimethylsilyl derivatives of flavonoids was compiled. TOFMS coupled to GC×GC enabled satisfactory identification of flavonoids in complex matrix samples at their LOD over a range of 0.5-10 μg/mL. Detection of all compounds was based on full-scan mass spectra and for each compound a characteristic ion was chosen for further quantification. This study shows that GC×GC-TOFMS yields high specificity for flavonoids derived from real natural samples, dark chocolate, propolis, and chrysanthemum.
研究了全二维气相色谱（GC×GC）在黄酮类化合物分析中的适用性，通过分离和鉴定标准品和复杂基质天然样品中的黄酮类化合物来进行。优化了调制温度以实现最佳分离和信号增强。比较了两种互补柱组上黄酮类化合物的三甲基硅烷（TMS）衍生物的分离模式。虽然 BPX5/BPX50（NP/P）柱组提供了更好的整体分离效果，但 BPX50/BPX5（P/NP）提供了更好的峰形和灵敏度。在黄酮类混合物上，对 GC×GC-TOFMS 与 NIST05 MS 库和实验室（内部创建）TOFMS 库的鉴定能力进行了比较。建立了具有非极性固定相的高性能毛细管柱的基本保留指数信息，并编制了黄酮类化合物 TMS 衍生物的质谱数据库。GC×GC-TOFMS 可在 0.5-10μg/mL 的范围内以 LOD 对复杂基质样品中的黄酮类化合物进行满意的鉴定。所有化合物的检测均基于全扫描质谱，并且为每个化合物选择了一个特征离子用于进一步定量。本研究表明，GC×GC-TOFMS 对来自真实天然样品、黑巧克力、蜂胶和菊花的黄酮类化合物具有高特异性。
