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固相采集法就是萃取物采集到填充柱中,填充柱中装有吸附材料[如:十八烷基硅石(ODS)]或惰性材料(如:不锈钢珠),固相采集也是一种比较常用的方法, 采集完成后,用适合的溶剂将产物从固相中洗脱下来[93~96,87]。在15℃时,用ODS阱采集蛇麻草中的精油和苦味素,用乙腈洗脱保留的化合物[30]。ODS 固体阱在低温也能有效的吸附挥发性物质,通过升温至45℃用有机溶剂洗脱这些化合物[30]。固相采集可以根据萃取物的性质选择适合的吸附阱及洗脱剂,并可以进一步提高选择性。例如:采用硅胶柱收集极性化合物,选用了合适的溶剂洗脱,就能得到满意的萃取率[94,96]。但是固相采集法也有它的局限性,如果选择了不适合的提携剂,可能导致萃取产物的丢失,因为提携剂通过吸附阱可能将产物洗掉,这种情况就应该选用溶剂法收集或用空瓶收集。此外,固相采集完成后,洗脱剂的选择非常重要,不适合的洗脱剂会影响萃取结果[28]。 在线采集法,即采集装置与其他分析方法的在线联用。采集装置与气相色谱相连,也就是超临界二氧化碳流体萃取-气相色谱联用技术是最成功的一种模式,是分析挥发性化合物的一个有用的方法。Smith 等[96]发现,低温(-10℃)采集对保留挥发性成分是必需的,即在低温条件下富集挥发性化合物,然后高温下使其蒸发。 除了超临界二氧化碳流体萃取—气相色谱联用技术外,其他的在线耦合方法也有报道[47,97],如:超临界二氧化碳流体萃取-液相色谱联用、超临界二氧化碳流体萃取-红外联用、超临界二氧化碳流体萃取-质谱联用等。Ramsey 等[98]采用超临界二氧化碳流体萃取-液相色谱-质谱联用,成功地分析了痕量的成分。和前2种方法相比联用技术有较高的灵敏度、较小的标准偏差、节省时间,而且对分析挥发性化合物非常有效,但是也存在许多不足之处,如对样品进样量的限制,色谱系统易被污染等等[99]。 7 结论 本文从超临界流体的选择、提携剂的选取、样品的制备、萃取温度和压力的影响、萃取物的采集等在超临界二氧化碳流体萃取实际操作中涉及到的几个方面进行了综述。随着中药现代化进程的加快,超临界流体萃取技术以其快速、提取率高、对环境污染小等特点,将在天然植物的提取中得到更加广泛的应用。 【参考文献】 1 王可成.中成药研究,1988,2:7-9. 2 Hannay JB, Hogarth J, Proc R.London A,1879,29,324. 3 杨涛,李静海.化工冶金, 1997,18(4):377-383. 4 Rein J, Cork CM, Furton KG. 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