Method for extracting huperzine a from huperzia serrata

Abstract

A method for extracting huperzine a from huperzia serrata comprises procedures including dilute acid soaking, repeated ultrasonic assisted extraction, repeated dilute acid and dilute alkali extraction, impurity removal by the aid of activated carbon, multiple times of low temperature recrystallization, and the like. The method has the advantages that alkaloid can be converted into alkaloid salt so as to be dissolved out by means of the dilute acid soaking procedure, cell walls of the huperzia serrata can be broken by means of the ultrasonic assisted extraction procedure in an extracting process, so that the alkaloid can be dissolved into soaking liquid better, and recovery rate is improved. Upon testing, the recovery rate of the huperzine a extracted by the method can reach 98.3%. Dilute acid and dilute alkali are used for extracting and re-extracting, so that impurities can be removed well and then are further removed better by the activated carbon, finally, residual impurities are removed by means of the repeated low temperature recrystallization procedure, and accordingly the high-purity huperzine a can be obtained. An embodiment detects that the purity of the extracted huperzine a reaches 99.11% HPLC (high performance liquid chromatography).

Description

technical field

[0001] The invention relates to a method for extracting alkaloids, in particular to a method for extracting huperzine A from Melaleuca huperzine. Background technique

[0002] The Melaleuca Pagoda is a fern of the genus Huperzia in the family Huperzaceae, also known as Huperzia serrata and King of Help. It is mainly distributed in the Northeast, the Yangtze River Basin and Fujian, Guangdong, Guangxi, Yunnan, Guizhou and other provinces. Folks often use the whole herb as medicine, which is poisonous and used for reducing fever, hemostasis, reducing swelling and detoxification, and traumatic injuries. The alkaloid huperzine A (HupA) contained in Melaleuca is an acetylcholinesterase inhibitor with the advantages of low toxicity, high efficiency, reversibility and high selectivity. curative effect, and has a certain effect on inhibiting organophosphate poisoning. Due to its unique medicinal value, Melaleuca and its extracts are increasingly being widely valued...

Examples

Embodiment 1

[0023] Cleanly select 100kg of Melaleuca medicinal materials, pulverize, the particle size is 10-20 mesh, and sieve. Add 2000L of 0.8% hydrochloric acid solution, soak for 60 minutes, then use 600W ultrasonic power to extract for 15 minutes, and then soak for 60 minutes. Then centrifuge with a centrifuge and take the supernatant. Add the filter residue to 1800L of 0.8% hydrochloric acid solution, soak for 45 minutes, then use 600W ultrasonic power to extract for 10 minutes, and then soak for 45 minutes. Then centrifuge with a centrifuge and take the supernatant. The two supernatants were combined, and the filtrate was concentrated to 1000 L with a rotary evaporator. Then add 10% ammonia water to adjust the pH value to 9-10, add 17L chloroform and mix with the concentrated solution, extract 4 times, combine the chloroform phase, and extract once more. Concentrate to 100L with a rotary evaporator to obtain Huperzia total alkaloids in chloroform concentrate. Then 100 L of 1% ...

Embodiment 2

[0026] Cleanly select 100kg of Melaleuca medicinal materials, pulverize, the particle size is 10-20 mesh, and sieve. Add 2500L of 0.8% hydrochloric acid solution, soak for 60 minutes, then use 600W ultrasonic power to extract for 15 minutes, and then soak for 60 minutes. Then centrifuge with a centrifuge and take the supernatant. Add the filter residue to 2200L of 0.8% hydrochloric acid solution, soak for 45 minutes, then use 600W power ultrasonic extraction for 10 minutes, and then soak for 45 minutes. Then centrifuge with a centrifuge and take the supernatant. The two supernatants were combined, and the filtrate was concentrated to 1000 L with a rotary evaporator. Then add 10% ammonia water to adjust the pH value to 10, add 17L chloroform and mix with the concentrated solution, extract 4 times, combine the chloroform phase, and extract once more. Concentrate to 100L with a rotary evaporator to obtain Huperzia total alkaloids in chloroform concentrate. Then 100 L of 1% Na...

Embodiment 3

[0029]Cleanly select 100kg of Melaleuca medicinal materials, pulverize, the particle size is 10-20 mesh, and sieve. Add 2200L of 0.8% hydrochloric acid solution, soak for 60 minutes, then use 600W ultrasonic power to extract for 15 minutes, and then soak for 60 minutes. Then centrifuge with a centrifuge and take the supernatant. Add the filter residue to 2000L of 0.8% hydrochloric acid solution, soak for 45 minutes, then use 600W ultrasonic power to extract for 10 minutes, and then soak for 45 minutes. Then centrifuge with a centrifuge and take the supernatant. The two supernatants were combined, and the filtrate was concentrated to 1000 L with a rotary evaporator. Then add 10% ammonia water to adjust the pH value to 10, add 17L chloroform and mix with the concentrated solution, extract 4 times, combine the chloroform phase, and extract once more. Concentrate to 100L with a rotary evaporator to obtain Huperzia total alkaloids in chloroform concentrate. Then 100 L of 1% NaH...

technical field

[0001] The invention relates to a method for extracting alkaloids, in particular to a method for extracting huperzine A from Melaleuca huperzine. Background technique

[0002] The Melaleuca Pagoda is a fern of the genus Huperzia in the family Huperzaceae, also known as Huperzia serrata and King of Help. It is mainly distributed in the Northeast, the Yangtze River Basin and Fujian, Guangdong, Guangxi, Yunnan, Guizhou and other provinces. Folks often use the whole herb as medicine, which is poisonous and used for reducing fever, hemostasis, reducing swelling and detoxification, and traumatic injuries. The alkaloid huperzine A (HupA) contained in Melaleuca is an acetylcholinesterase inhibitor with the advantages of low toxicity, high efficiency, reversibility and high selectivity. curative effect, and has a certain effect on inhibiting organophosphate poisoning. Due to its unique medicinal value, Melaleuca and its extracts are increasingly being widely valued...

Examples

Embodiment 1

[0023] Cleanly select 100kg of Melaleuca medicinal materials, pulverize, the particle size is 10-20 mesh, and sieve. Add 2000L of 0.8% hydrochloric acid solution, soak for 60 minutes, then use 600W ultrasonic power to extract for 15 minutes, and then soak for 60 minutes. Then centrifuge with a centrifuge and take the supernatant. Add the filter residue to 1800L of 0.8% hydrochloric acid solution, soak for 45 minutes, then use 600W ultrasonic power to extract for 10 minutes, and then soak for 45 minutes. Then centrifuge with a centrifuge and take the supernatant. The two supernatants were combined, and the filtrate was concentrated to 1000 L with a rotary evaporator. Then add 10% ammonia water to adjust the pH value to 9-10, add 17L chloroform and mix with the concentrated solution, extract 4 times, combine the chloroform phase, and extract once more. Concentrate to 100L with a rotary evaporator to obtain Huperzia total alkaloids in chloroform concentrate. Then 100 L of 1% ...

Embodiment 2

[0026] Cleanly select 100kg of Melaleuca medicinal materials, pulverize, the particle size is 10-20 mesh, and sieve. Add 2500L of 0.8% hydrochloric acid solution, soak for 60 minutes, then use 600W ultrasonic power to extract for 15 minutes, and then soak for 60 minutes. Then centrifuge with a centrifuge and take the supernatant. Add the filter residue to 2200L of 0.8% hydrochloric acid solution, soak for 45 minutes, then use 600W power ultrasonic extraction for 10 minutes, and then soak for 45 minutes. Then centrifuge with a centrifuge and take the supernatant. The two supernatants were combined, and the filtrate was concentrated to 1000 L with a rotary evaporator. Then add 10% ammonia water to adjust the pH value to 10, add 17L chloroform and mix with the concentrated solution, extract 4 times, combine the chloroform phase, and extract once more. Concentrate to 100L with a rotary evaporator to obtain Huperzia total alkaloids in chloroform concentrate. Then 100 L of 1% Na...

Embodiment 3

[0029]Cleanly select 100kg of Melaleuca medicinal materials, pulverize, the particle size is 10-20 mesh, and sieve. Add 2200L of 0.8% hydrochloric acid solution, soak for 60 minutes, then use 600W ultrasonic power to extract for 15 minutes, and then soak for 60 minutes. Then centrifuge with a centrifuge and take the supernatant. Add the filter residue to 2000L of 0.8% hydrochloric acid solution, soak for 45 minutes, then use 600W ultrasonic power to extract for 10 minutes, and then soak for 45 minutes. Then centrifuge with a centrifuge and take the supernatant. The two supernatants were combined, and the filtrate was concentrated to 1000 L with a rotary evaporator. Then add 10% ammonia water to adjust the pH value to 10, add 17L chloroform and mix with the concentrated solution, extract 4 times, combine the chloroform phase, and extract once more. Concentrate to 100L with a rotary evaporator to obtain Huperzia total alkaloids in chloroform concentrate. Then 100 L of 1% NaH...

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