Smith R D, Udseth H R, Wright B W
J Chromatogr Sci. 1985 May;23(5):192-9. doi: 10.1093/chromsci/23.5.192.
The potential application of capillary column supercritical fluid chromatography (SFC) and SFC/mass spectrometry (SFC/MS) for the separation and analysis of mycotoxins of the trichothecene group was examined. Trichothecenes present significant analytical problems for both gas and liquid chromatography with a major difficulty for the latter being the lack of sufficiently sensitive and selective detectors. Supercritical carbon dioxide mobile phases at temperatures up to 100 degrees C were used with deactivated fused silica columns coated with crosslinked stationary phases. Separations were obtained under pressure ramped conditions using long (15 m) 50-micron i.d. columns for several trichothecenes (diacetoxyscirpenol, deoxynivalenol, and T-2 toxin) and related higher molecular weight macrocyclic (roridin and verrucarin) trichothecenes. In addition, new rapid pressure programming techniques with short (less than 2m) 25- to 50-micron i.d. capillary columns were used to obtain fast separations in as little as 1 min. SFC/MS with ammonia chemical ionization provided high selectivity and sensitive detection (with approximately 1-pg detection limits) for trichothecene mixtures. The extension to complex sample matrices is discussed and the application of selective MS/MS detection is demonstrated.
考察了毛细管柱超临界流体色谱法（SFC）和SFC/质谱法（SFC/MS）在分离和分析单端孢霉烯族霉菌毒素方面的潜在应用。单端孢霉烯族毒素给气相色谱法和液相色谱法都带来了重大的分析难题，液相色谱法的主要困难在于缺乏足够灵敏和选择性的检测器。使用温度高达100℃的超临界二氧化碳流动相，搭配涂覆有交联固定相的去活熔融石英柱。在压力梯度条件下，使用长15米、内径50微米的柱对几种单端孢霉烯族毒素（二醋酸雪腐镰刀菌烯醇、脱氧雪腐镰刀菌烯醇和T-2毒素）以及相关的高分子量大环（肉毒素和疣孢菌素）单端孢霉烯族毒素进行分离。此外，采用内径25至50微米、长度小于2米的短毛细管柱的新型快速程序升压技术，可在短短1分钟内实现快速分离。采用氨化学电离的SFC/MS对单端孢霉烯族毒素混合物具有高选择性和灵敏检测能力（检测限约为1皮克）。讨论了向复杂样品基质的扩展，并展示了选择性MS/MS检测的应用。
