白术生、制品的DCBI-MS鉴别

Identification of raw and processed atractylodes by DCBI-MS

目的:建立白术生、制品的解吸附电晕束离子化质谱(DCBI-MS)(秒级)快速鉴别方法。方法:采用原位跟踪技术跟踪苍术酮的转化,初步探讨白术的最佳炮制温度;采用DCBI-MS法对白术生、制品的化学成分进行分析。结果 :白术最佳的炮制温度为120~140℃。60批样品中包括对照药材1批,生药材27批,土炒白术19批,麸炒白术13批;与生品相比较,加热炮制品中苍术酮的含量均有不同程度的降低,白术内酯Ⅱ(atractylenolideⅡ)和白术内酯Ⅲ(atractylenolideⅢ)的相对响应丰度值有显著增高;生白术的相似度为0.90~0.95,土炒白术的相似度为0.83~0.90,而麸炒白术的相似度为0.71~0.82,且可直观地将白术生品、土炒白术和麸炒白术分为三类。结论:DCBI-MS法可有效跟踪炮制过程中苍术酮向白术内酯(atractylenolide)Ⅰ~Ⅲ转化的情况,获得其最佳炮制参数,并可有效辨别白术生、制品,可作为炮制条件优化的快速检测工具,为中药材的质量控制提供参考。

Objective:To establish a rapid identification method for desorption corona beam ionization-mass spectrometry(DCBI MS)(second order) of processed and unprocessed atractylodes. Methods:The in situ tracking technique was used to track the transformation of atrsctyl ketone,and the best processing temperature of atrectylodes were discussed. The chemical constituents of processed and unprocessed atractylodes were analyzed by DCBI-MS. Results:The bestprocessing temperature of atractylodes were 120-140 ℃. Sixty batches of samples included 1 batch of reference medicinal materials,27 batches of raw medicinal herbs,19 batches of earth-boiled atractylodes,and 13 batches of bran-enriched atractylodes;compared with raw products,the contents of atractyl ketone in processed products decreased to varying degrees,and the relative abundance of atractylenolide Ⅰ and atractylenolide Ⅰ increased significantly;the similarity of raw atractylodes was 0.90-0.95, the similarity of atraetylodes processed with soil was 0.83-0.90,and the similarity of atractylodes processed with wheat bran was 0.71-0.82,and it can be used to visually distinguish between raw atractylodes,atractylodes processed with soil,and atractylodes processed with wheat bran. Conclusion:The DCBI-MS method can effectively track the transformation of atractylenolide Ⅰ,I and I during processing. and obtain the best processing parameters,and can effectively distinguish the processed and unprocessed atractylodes,which can be optimized as processing conditions. The rapid detection tool provides a reference for the quality control of Chinese herbal medicines.