目的 建立银翘散蒸馏液中主要挥发性成分的含量测定方法,比较银翘散煮散与饮片煎煮过程中挥发性成分的蒸发规律,为客观表征银翘散"香气大出即取服"煎煮终点判断方法提供科学依据。方法 收集不同煎煮时间段银翘散煮散与饮片煎煮蒸馏液,采用GC-MS法定性分析挥发性成分并测定α-蒎烯、(−)-β-蒎烯、月桂烯、对伞花烃、(R)-(+)-柠檬烯、γ-松油烯、薄荷酮、薄荷醇、4-萜烯醇、(R)-(+)-胡薄荷酮、(+)-香芹酮、胡椒酮12种主要挥发性成分的含量,比较不同煎煮时间银翘散煮散与饮片挥发性成分蒸发速度。结果 银翘散煮散与饮片挥发油GC-MS总离子流色谱图分别确定48和34个色谱峰,其中相对质量分数大于0.5%的色谱峰分别为26、21个;随着煎煮时间的延长,煮散蒸馏液中,12种成分的平均蒸发速度均先增加后减少,均在煮沸0~10 min达到最大值,分别为7.28、13.21、1.06、0.48、1.49、0.42、2.08、2.27、1.76、0.79、0.16、0.20 mg/min;饮片蒸馏液中,α-蒎烯、(−)-β-蒎烯、月桂烯、对伞花烃、(R)-(+)-柠檬烯、γ-松油烯的平均蒸发速度先增加后趋于平缓,在25~30 min达到最大值,分别为1.38、4.58、0.11、0.06、0.22、0.04 mg/min,其余6种成分则先增加后减少,在0~5 min达到最大值,分别为1.30、2.21、0.42、0.92、0.26、0.37 mg/min。结论 煎煮时间与药材粒度对银翘散挥发性成分蒸发速度影响较大;相比于饮片煎煮,煮散挥发性成分蒸发速度更快,煮沸约5 min时,12种主要挥发性成分均达到最大值,煮沸约15 min后,12种挥发性成分蒸发速度均明显减小,提示银翘散"香气大出即取服"传统煎煮方法煎煮终点为煮沸5 min左右,以饮片煎煮的银翘散类方制剂挥发性成分的蒸发规律与煮散具有一定差异性。

Objective To establish a method for the determination of main volatile components in Yinqiao Powder (银翘散) distillate and compare the evaporation law of volatile components between the process of powder and pieces decoction, so as to provide an evidence for objectively characterizing the boiling endpoint of its traditional decocting method "taking when the fragrance volatilized fiercely". Methods Powder and pieces distillates with different decocting time were prepared to study the dynamic changes of chemical components during decocting process. GC-MS was used to analyze the volatile components qualitatively and determine the contents of α-pinene, (−)-β-pinene, myrcene, p-cymene, (R)-(+)-limonene, γ-terpinene, menthone, menthol, terpinen-4-ol, (R)-(+)-pulegone, D-carvone and piperitone in powder and pieces distillates. Results A total of 48 and 34 chromatographic peaks were detected in GC-MS total ion chromatograms of volatile oil from powder and pieces, of which 26 and 21 peaks with relative mass fraction were greater than 0.5%, respectively. With the extension of the boiling time, the evaporation rates of 12 components in the decocting distillate all increased to maximum and then decreased. When boiling for 0-10 min, the maximum average evaporation rates were 7.28, 13.21, 1.06, 0.48, 1.49, 0.42, 2.08, 2.27, 1.76, 0.79, 0.16 and 0.20 mg/min, respectively. In the distillate of pieces, the evaporation rates of α-pinene, (−)-β-pinene, myrcene, p-cymene, (R)-(+)-limonene and γ-terpinene all increased to maximum and then tended to be flat. When boiling for 25-30 min, the maximum average evaporation rates were 1.38, 4.58, 0.11, 0.06, 0.22 and 0.04 mg/min, respectively. The other six components increased first and then decreased, and reached the maximum value in 0-5 min, which were 1.30, 2.21, 0.42, 0.92, 0.26 and 0.37 mg/min, respectively. Conclusion The decocting time and particle size of raw medicinal materials had great effects on the evaporation rate of volatile components of Yinqiao Powder; compared with pieces, the evaporation rate of volatile components in powder decoction was faster. When boiling for about 5 min, 12 main volatile components reach the maximum. After boiling for about 15 min, the evaporation rate of 12 volatile components decreases significantly, indicating that the traditional decoction method of Yinqiao Powder "taking when the fragrance volatilized fiercely" has a boiling end point of about 5 min. However, the evaporation law of volatile components in pieces decoction is different from that in powder decoction.

R283.6

国家自然科学基金资助项目（81760711）；江西省自然科学基金资助项目（20192ACBL21033）