蒲黄炒炭前后亲脂性成分的GC-MS分析

目的:探讨蒲黄炒炭前后亲脂性成分的变化。方法:将生蒲黄和蒲黄炭分别用石油醚(60～90℃)连续回流提取,提取物甲酯化后进行气相色谱-质谱联用(GC-MS)分析,并利用NIST谱库检索鉴定化合物,用归一化法计算各化合物的相对百分含量。结果:从生蒲黄和蒲黄炭石油醚提取物中鉴定了32个化合物,其中相同化合物20个、不同化合物各6个。在相同化合物中,炮制后相对百分含量显著增加的有3-甲基-2-丁烯酸-2-苯乙基酯、己二酸二甲酯、邻苯二甲酸二甲酯、邻苯二甲酸二乙酯、二苯胺、癸二酸二甲酯、邻苯二甲酸甲基乙基酯、邻苯二甲酸甲基-2-乙基己基酯、邻苯二甲酸二异辛酯等,炮制后相对百分含量显著降低的有壬二酸二甲酯、邻苯二甲酸二异丁酯、3,5-二烯豆甾烷等;在不同化合物中,生蒲黄有而在蒲黄炭中没有检测到的化合物是8-羟基辛酸甲酯、9-羟基壬酸甲酯、10-十八碳烯酸甲酯、间羟基肉桂酸甲酯、3-4-(乙酰氧基)-3-甲氧基苯基]-2-丙烯酸甲酯、11-十八碳烯酸甲酯等,蒲黄炭有而生蒲黄中没有检测到的化合物是3-羟基-螺甾-8-烯-11-酮、氢化肉桂酸甲酯、2,4-二甲基己二酸、2,4-二叔丁基苯酚、十一碳二酸二甲酯、9,10-二羟基硬脂酸甲酯等。结论:蒲黄炒炭前后亲脂性成分种类和含量都有一定程度的变化,但是化合物类型变化不大。

GC-MS analysis of the fatty components of Pollen Typhae before and after being carbonized

OBJECTIVE: To study the changes of the fatty components of Pollen Typhae before and after being carbonized. Method: Pollen Typhae and Pollen Typhae carbonisatus were extracted with petroleum ether (60-90 degrees C) respectively. The two kinds of extracts were analyzed by GC-MS after saponificated and methanolized, and their constituents were searched through NIST. The contents of the constituents were determined by method of normalization. RESULT: Either in Pollen Typhae or in Pollen Typhae carbonisatus, 32 components were identified, among which 20 components were the same and 6 were different respectively. Among the same components, the relative contents of 3-methyl-2-butenoic acid-2-phenylethyl ester, hexanedioic acid-dimethyl ester, dimethyl phthalate, diethyl phthalate, diphenylamine, sebacic acid dimethyl ester, 1,2-benzenedicarboxylic acid, ethyl methyl ester, methyl-2-ethylhexyl phthalate and diisooctyl phthalate etc. increased obviously, and the relative contents of nonanedioic acid-dimethyl ester, diisobutyl phthalate and stigmastan-3,5-dien etc. decreased greatly. Among the different components, 8-hydroxy-octanoic acid-methyl ester, 9-hydroxy-nonanoic acid-methyl ester, 10-octadecenoic acid-methyl ester, m-hydroxycinnamic acid-methyl ester,3-4-( acetyloxy)-3-methoxyphenyl]2-propenoic acid-methyl ester and 11-octadecenoic acid-methyl ester were detected in Pollen Typhae, 3-hydroxyspirost-8-en-11-one, benzenepropanoic acid-methyl ester, 2,4-dimethylhexanedioic acid; 2,4-bis (1,1-dimethylethyl)-phenol, undecanedioic acid-dimethyl ester and 9,10-dihydroxy-octadecanoic acid-methyl ester were detected in Pollen Typhae carbonistatus. CONCLUSION: The species and contents of the fatty components in Pollen Typhae changed before and after being carbonized, but their chemical types didn't change too much.