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目的:从中药麻黄所含阿魏酰组胺和麻黄根碱的结构以及可能的生源关系推测其尚有未被发现的组胺、腐胺、亚精胺和精胺等成分,建立柱前衍生化RP-HPLC法测定麻黄及麻黄根中11种生物胺。方法:药材样品经1 mol·L-1盐酸提取,正丁醇-二氯甲烷(1∶1)萃取富集,以丹磺酰氯为柱前衍生试剂进行衍生化,RP-HPLC法测定。采用Shimadzu C18色谱柱(200mm×4.6 mm,5μm),以乙腈(A)-水(B)为流动相,梯度洗脱(0~7 min,45%A→50%A;7~25 min,50%A→90%A;25~35min,90%A;35~40 min,90%A→45%A),流速为0.8 m L·min-1,检测波长为254 nm,柱温为30℃。结果:甲胺、尸胺、组胺、亚精胺与精胺的线性范围为0.10~10.00 mg·L-1(r>0.999),色胺、腐胺的线性范围为0.10~50.00 mg·L-1(r>0.999),2-苯乙胺、5-羟色胺、酪胺与多巴胺的线性范围为0.25~10.00 mg·L-1(r>0.999),平均回收率在75.6%~101.1%之间。麻黄中含有甲胺、色胺、腐胺、尸胺、组胺、亚精胺、多巴胺与精胺。麻黄根中含有甲胺、腐胺、尸胺、组胺、亚精胺与精胺。结论:经方法学验证,该方法可用于测定麻黄中甲胺、色胺、2-苯乙胺、腐胺、尸胺、组胺、5-羟色胺、酪胺、亚精胺、多巴胺与精胺11种生物胺类成分。这是首次发现在麻黄中含有生物胺类成分,同时也证实了麻黄中存在组胺、腐胺、精胺和亚精胺的推测,并为其生源关系提供了证据。该研究方法也可用于其他中药或天然药物化学成分的深入研究。
OBJECTIVE: To determine the existence of undetected histamine, putrescine, spermidine and spermine among the structures of ferulic acid and ephedrine contained in Chinese ephedra, Determination of 11 biogenic amines in ephedra and ephedra roots by RP-HPLC. Methods: The medicinal samples were extracted with 1 mol·L-1 hydrochloric acid, extracted with n-butanol-methylene chloride (1: 1) and derivatized with dansyl chloride as the pre-column derivatization reagent and determined by RP-HPLC. The mobile phase was eluted with a gradient of Shimadzu C18 column (200 mm × 4.6 mm, 5 μm) using acetonitrile (A) -water (B) as mobile phase (0-7 min, 45% A → 50% A; 7-25 min, 50% A → 90% A; 25-35 min, 90% A; 35-40 min, 90% A → 45% A) at a flow rate of 0.8 m L · min-1 with a detection wavelength of 254 nm and a column temperature of 30 ℃. Results: The linear ranges of methylamine, cadaverine, histamine, spermidine and spermine were 0.10-10.00 mg · L-1 (r> 0.999). The linear ranges of tryptamine and putrescine were 0.10-50.00 mg · L (R> 0.999). The linear range of 2-phenethylamine, serotonin, tyramine and dopamine was 0.25-10.00 mg · L -1 (r> 0.999) .The average recoveries ranged from 75.6% to 101.1% between. Ephedrine contains methylamine, tryptamine, putrescine, cadaverine, histamine, spermidine, dopamine and spermine. Ephedrine root contains methylamine, putrescine, cadaverine, histamine, spermidine and spermine. Conclusion: The method can be used for the determination of methylamine, tryptamine, 2-phenylethylamine, putrescine, cadaverine, histamine, serotonin, tyramine, spermidine, dopamine and spermine Eleven biogenic amine components. This is the first discovery of biogenic amines in Ephedra, and also confirms the presence of histamine, putrescine, spermine and spermidine in ephedra and provides evidence for their association with their sources. The research method can also be used for further study of the chemical composition of other traditional Chinese medicine or natural medicine.