Method for extracting sinomenine hydrochloride from caulis sinomenii

Abstract

The invention discloses a method for extracting sinomenine hydrochloride from caulis sinomenii. The method comprises the following steps: crushing sinomenium acutum roots; sieving by a 40-mesh sieve; adding 5-8 times of a 60-70% ethanol liquid; extracting for 1-2 hours in a double frequency ultrasonic device; filtering and decompressing and concentrating; and purifying the filtrate by virtue of column chromatography on silica gel to obtain high purity sinomenine hydrochloride. The method disclosed by the invention is simple in process and high is recovery rate and the separated sinomenine hydrochloride is high in purity.

Description

technical field

[0001] The invention relates to a method for extracting sinomenine from Caulis chinensis, belonging to the technical field of natural medicines. Background technique

[0002] Qingfengteng is the dried rhizome of Qingteng and Maoqingteng of Fangjiaceae plants. It has the effects of dispelling rheumatism, dredging meridians, and urinating. It is used to treat rheumatic arthralgia, joint swelling, paralysis and itching. The main content of Qingfengteng is sinomenine, and it also contains bisinomenine, magnolanine, and tetrandrine. Sinomenine, the molecular formula is C 19 h 23 NO 4 , molecular weight 329.38, filamentous crystal, melting point 161°C, easily soluble in chloroform, acetone, ethanol and lye, slightly soluble in water and ether. Sinomenine has anti-inflammatory, immunosuppressive, analgesic, hypotensive, anti-arrhythmic and other pharmacological effects. In recent years, with the increasing incidence of rheumatism, rheumatoid arthritis, limb pai...

Examples

Embodiment 1

[0013] Crush the root of Teng chinensis, pass through a 40-mesh sieve, add 5 times of 70% ethanol solution, in a dual-frequency ultrasonic device, the ultrasonic frequency is 20Hz, 40Hz, and the ultrasonic power is 500W, extract for 2 hours, filter, and concentrate under reduced pressure. The filtrate was added to a silica gel column, and the chloroform-methanol with a volume ratio of 1:1 was eluted, and the flow rate of the eluent was 2.5ml / min. The eluate was collected, and the collected eluate was tracked and detected by high performance liquid chromatography. The eluate was recovered by a rotary evaporator to recover the solvent to obtain sinomenine with an extraction rate of 79.8% and a purity of 96.8%.

Embodiment 2

[0015] Grind the root of Teng chinensis, pass through a 40 mesh sieve, add 8 times of 60% ethanol solution, in a dual-frequency ultrasonic device, the ultrasonic frequency is 20Hz, 40Hz, and the ultrasonic power is 600W, extract for 1.5h, filter, and concentrate under reduced pressure , the filtrate was added to the silica gel column, and the volume ratio was 1:1 for chloroform-methanol elution, and the eluent flow rate was 2.0ml / min, and the eluent was collected, and the collected eluent was tracked and detected by high performance liquid chromatography, The eluents were combined, and the solvent was recovered by a rotary evaporator to obtain sinomenine with an extraction rate of 85.8% and a purity of 98.2%.

Embodiment 3

[0017] Crush the root of Teng chinensis, pass through a 40-mesh sieve, add 6 times of 65% ethanol solution, in a dual-frequency ultrasonic device, the ultrasonic frequency is 20Hz, 40Hz, and the ultrasonic power is 550W, extract for 1h, filter, and concentrate under reduced pressure. The filtrate was added to a silica gel column, and the chloroform-methanol with a volume ratio of 1:1 was eluted, and the flow rate of the eluent was 1.5ml / min. The eluate was collected, and the collected eluate was detected by high performance liquid chromatography, and the combined The eluate was recovered by a rotary evaporator to recover the solvent to obtain sinomenine with an extraction rate of 80.3% and a purity of 97.6%.

technical field

[0001] The invention relates to a method for extracting sinomenine from Caulis chinensis, belonging to the technical field of natural medicines. Background technique

[0002] Qingfengteng is the dried rhizome of Qingteng and Maoqingteng of Fangjiaceae plants. It has the effects of dispelling rheumatism, dredging meridians, and urinating. It is used to treat rheumatic arthralgia, joint swelling, paralysis and itching. The main content of Qingfengteng is sinomenine, and it also contains bisinomenine, magnolanine, and tetrandrine. Sinomenine, the molecular formula is C 19 h 23 NO 4 , molecular weight 329.38, filamentous crystal, melting point 161°C, easily soluble in chloroform, acetone, ethanol and lye, slightly soluble in water and ether. Sinomenine has anti-inflammatory, immunosuppressive, analgesic, hypotensive, anti-arrhythmic and other pharmacological effects. In recent years, with the increasing incidence of rheumatism, rheumatoid arthritis, limb pai...

Examples

Embodiment 1

[0013] Crush the root of Teng chinensis, pass through a 40-mesh sieve, add 5 times of 70% ethanol solution, in a dual-frequency ultrasonic device, the ultrasonic frequency is 20Hz, 40Hz, and the ultrasonic power is 500W, extract for 2 hours, filter, and concentrate under reduced pressure. The filtrate was added to a silica gel column, and the chloroform-methanol with a volume ratio of 1:1 was eluted, and the flow rate of the eluent was 2.5ml / min. The eluate was collected, and the collected eluate was tracked and detected by high performance liquid chromatography. The eluate was recovered by a rotary evaporator to recover the solvent to obtain sinomenine with an extraction rate of 79.8% and a purity of 96.8%.

Embodiment 2

[0015] Grind the root of Teng chinensis, pass through a 40 mesh sieve, add 8 times of 60% ethanol solution, in a dual-frequency ultrasonic device, the ultrasonic frequency is 20Hz, 40Hz, and the ultrasonic power is 600W, extract for 1.5h, filter, and concentrate under reduced pressure , the filtrate was added to the silica gel column, and the volume ratio was 1:1 for chloroform-methanol elution, and the eluent flow rate was 2.0ml / min, and the eluent was collected, and the collected eluent was tracked and detected by high performance liquid chromatography, The eluents were combined, and the solvent was recovered by a rotary evaporator to obtain sinomenine with an extraction rate of 85.8% and a purity of 98.2%.

Embodiment 3

[0017] Crush the root of Teng chinensis, pass through a 40-mesh sieve, add 6 times of 65% ethanol solution, in a dual-frequency ultrasonic device, the ultrasonic frequency is 20Hz, 40Hz, and the ultrasonic power is 550W, extract for 1h, filter, and concentrate under reduced pressure. The filtrate was added to a silica gel column, and the chloroform-methanol with a volume ratio of 1:1 was eluted, and the flow rate of the eluent was 1.5ml / min. The eluate was collected, and the collected eluate was detected by high performance liquid chromatography, and the combined The eluate was recovered by a rotary evaporator to recover the solvent to obtain sinomenine with an extraction rate of 80.3% and a purity of 97.6%.