提出了动物肝组织中雷公藤甲素与雷公藤酯甲的液相色谱-质谱法分析方法。用快速溶剂萃取仪用乙腈将动物肝组织中雷公藤甲素与雷公藤酯甲萃取到有机相,提取液经凝胶渗透色谱净化除去基质的干扰,所得洗脱液40 ℃氮吹挥干后用甲醇定容至0.5 mL,用液相色谱-质谱法测定。雷公藤甲素与雷公藤酯甲的质量浓度均在5~1 000 μg·L-1范围内呈线性,检出限(3S/N)均为1.0 μg·L-1。在动物肝组织中用标准加入法做回收及精密度试验,结果为:雷公藤甲素和雷公藤酯甲的回收率分别在69.3%~77.8%,73.1%~77.2%之间;雷公藤甲素和雷公藤酯甲测定值的相对标准偏差(n=5)分别在3.2%~3.3%,2.3%~3.0%之间。

A method for determination of triptolide and wilforlide A in animal liver by LC-MS was proposed. The animal liver tissue sample was extracted with acetonitrile, and the extract obtained was purified by gel permeation chromatography (GPC) to eliminate the interference of matrix. Eluate from the GPC column was evaporated to near dryness by N2-blowing at 40 ℃, and the residue was taken up with 0.5 mL of methanol, which was used for LC-MS determination. Linearity ranges of triptolide and wilforlide A were kept same between 5-1 000 μg·L-1, with same detection limits (3S/N) of 1.0 μg·L-1. Recovery and precision were tested by standard addition method and the results obtained were as follow: values of recovery in the ranges of 69.3%-77.8% for triptolide and 73.1%-77.2% for wilforlide A; values of RSD′s (n=5) in the ranges of 3.2%-3.3% for triptolide and 2.3%-3.0% for wilforlide A respectively.