CN105731524A - Method for extracting and separating mercury sulfide nanoparticles in Mongolian medicine Menggenwusu - Google Patents
Method for extracting and separating mercury sulfide nanoparticles in Mongolian medicine Menggenwusu Download PDFInfo
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Abstract
The invention relates to a method for extracting and separating mercury sulfide nanoparticles in a Mongolian medicine Menggenwusu, belonging to the field of active ingredient extraction of a traditional processed product of a Mongolian medicine. The method comprises extraction of mercury sulfide sample particles and differential separation of mercury sulfide micro-nanoparticles, wherein in the extraction, the mercury sulfide sample particles are extracted by xylene, and elemental sulfur in Menggenwusu is removed; and in the differential separation, the mercury sulfide micro-nanoparticles different in particle size can be obtained by controlling the PVP concentration, feed ratio, centrifuge speed and centrifugation time. By adopting the method provided by the invention, the extracted mercury sulfide micro-nanoparticles have high purity, stable composition and exact structure while clinical administration is more scientific; and moreover, with the separated mercury sulfide micro-nanoparticles different in particle size, the efficacy of the nanoparticles different in particle size can be compared.
Description
Technical field
The present invention relates to the extraction separation method of cinnabar nano-particle in a kind of mongolian medicine root in Meng Usu, belong to mongolian medicine tradition processed product extracts active ingredients field.
Background technology
Root in Meng Usu is that mercurous medical material commonly used by mongolian medicine, passes through the cinerous block to Lycoperdon polymorphum Vitt of complicated concocting process gained in 1:1 (firmly system) or the mixing of 1:2 (soft system) ratio also known as controlling the water circulation silver, mongolian medicine teacher's hydrargyrum and sulfur.Controlling the water circulation silver applicating history is long, pungent, cold, heavy, have severe toxicity, dry " Xieri Wusu Symptom ", parasite killing, and disappear " very breathing out ", can be used for rheumatoid, trip pain, psoriasis, tinea, anthrax, syphilis, etc. disease.
Root in Meng Usu is characteristic mongolian medicine root in Meng Usu 18 " monarch drug ", at autoimmune disease, as the treatment such as rheumatoid arthritis, psoriasis has clear and definite curative effect.Being good at by one of feature that hydrargyrum is mongolian medicine, hydrargyrum its toxicity after rationally concocting reduces, and drug effect increases.The concocted specification of controlling the water circulation silver, quality standard research achieve progress in recent years, but the research of root in Meng Usu effective ingredient and " attenuation synergistic " are reduced in mongolian medicine to the problems such as mercury content and there is no effective workaround.Root in Meng Usu is mainly composed of cinnabar and elemental sulfur, and cinnabar is to be embedded in sulfur with the form of micro-nano granule, form unique microstructure, separate cinnabar micro-nano granules significant for root in Meng Usu active substance basis and processing procedure Study on Modernization.
Summary of the invention
It is an object of the invention to provide the extraction separation method of cinnabar nano-particle in a kind of mongolian medicine root in Meng Usu, in mongolian medicine root in Meng Usu, cinnabar micro-nano granules is for object of study, it is carried out surname extraction, and is easily separated by cinnabar different-grain diameter by differential centrifugation.
It is an object of the invention to be achieved through the following technical solutions:
The extraction separation method of the cinnabar nano-particle in mongolian medicine root in Meng Usu, comprises the following steps:
Step 1, the extraction of cinnabar sample particle:
Step 1.1, weighs 1-5g root in Meng Usu powder and wraps with filter paper, putting in apparatus,Soxhlet's；
Step 1.2, is placed in round-bottomed flask by the organic solvent of 100-200ml, is heated backflow 4-10h, obtains cinnabar sample in described apparatus,Soxhlet's at 100-160 DEG C；
Step 1.3, cinnabar sample is taken out, is positioned in fume hood 10-24h and the organic solvent in cinnabar sample is volatilized, more described cinnabar sample is positioned in vacuum drying oven, at 50 DEG C, it is placed in drying baker and obtains cinnabar sample particle after dry 48 hours；
Step 2, the differential of cinnabar micro-nano granules separates:
Step 2.1, weighs the cinnabar sample particle of 1-5g, is dispersed in by described cinnabar sample particle in the PVP solution of 10-100mg/mL of 25ml, crosses Medium speed filter paper, respectively obtain the cinnabar granule on filtrate and Medium speed filter paper after ultrasonic disperse 30min；
Step 2.2, the cinnabar granule on described Medium speed filter paper, after deionized water and dehydrated alcohol wash 5 times respectively, is placed in vacuum drying oven, at 50 DEG C, dries and within 48 hours, obtains cinnabar 0# granule；
Step 2.3, proceed in the centrifuge tube of 10ml after described filtrate is stirred, after the centrifugal 3-10min of 1000rad/min, collect the suspension on described centrifuge tube top, described centrifuge tube adds described PVP solution, precipitation ultrasonic disperse bottom centrifuge tube is dissolved, continue with the centrifugal 3-10min of 1000rad/min, and the suspension on described centrifuge tube top is merged collection, repeatable operation 3-5 time, again by the precipitation bottom centrifuge tube after deionized water and dehydrated alcohol wash 5 times respectively, it is placed in vacuum drying oven, under 50 ° of C, dry and within 48 hours, obtain cinnabar 1# granule；
Step 2.4, proceeds in the centrifuge tube of 10ml by the suspension in step 2.3, repeats the operation of step 2.3, and centrifugal speed is brought up to 3000rad/min, obtain cinnabar 2# granule；
Step 2.5, the suspension in step 2.4 proceeds in the centrifuge tube of 10ml, repeats the operation of step 2.3, and centrifugal speed is brought up to 5000rad/min, obtain cinnabar 3# granule；
Step 2.6, the suspension in step 2.5 proceeds in the centrifuge tube of 10ml, repeats the operation of step 2.3, and centrifugal speed is brought up to 7000rad/min, obtain cinnabar 4# granule；
Step 2.7, the suspension in step 2.6 proceeds in the centrifuge tube of 10ml, repeats the operation of step 2.3, and centrifugal speed is brought up to 9000rad/min, obtain cinnabar 5# granule；
Step 2.8, the suspension in step 2.7 proceeds in the centrifuge tube of 10ml, repeats the operation of step 2.3, and centrifugal speed is brought up to 11000rad/min, obtain cinnabar 6# granule；
Wherein, the cinnabar micro-nano granules of described cinnabar 0# granule, described cinnabar 1# granule, described cinnabar 2# granule, described cinnabar 3# granule, described cinnabar 4# granule, described cinnabar 5# granule, described cinnabar 6# granule respectively different-grain diameter.
Further, in step 1.1, weigh 2g root in Meng Usu powder.
Further, in step 1.2, described organic solvent is dimethylbenzene, carbon tetrachloride, benzene or toluene.
Further, described organic solvent is dimethylbenzene.
Further, in step 1.2, at 150 DEG C, it is heated backflow 4-10h.
Further, in step 2.1, weigh dried cinnabar sample in 2g step 1.3.
Further, described PVP solution concentration is 40mg/mL.
Further, in step 2.3, centrifugation time is 5min.
Further, described root in Meng Usu powder size is less than or equal to 200 orders.
The invention have the benefit that
1, the method for the invention adopts the elemental sulfur in organic solvent extraction mongolian medicine root in Meng Usu, can efficiently separate two kinds of main components in crude drug, plays a key effect for material base research.
2, the method for the invention is extracted the purity height of cinnabar micro-nano granules, stable components, the clear and definite clinical application of structure are more scientific, the cinnabar micro-nano granules of the different-grain diameter of separation, it is possible to compare the drug effect of different-grain diameter nano-particle.
3, the method for the invention is simple, workable, it is easy to regulation and standardization, can be mass-produced.
4, adopting the method for the invention, between the yield 70-80% of cinnabar micro-nano granules, in the cinnabar granule of separation, cinnabar content can be increased to 97%-99%.And soluble mercury content drops to 1-2mg/g in sample, the size tunable system of granule is in 7 intervals, and each interval particle diameter is normal distribution.The cinnabar that nano-particle comprises structure respectively α and β type is detected through XRD.
Accompanying drawing explanation
Fig. 1 is electron scanning micrograph and the grain size distribution of the cinnabar micro-nano granules of the different-grain diameter that embodiment 1 is extracted；
The XRD figure spectrum of the cinnabar micro-nano granules of Fig. 2 embodiment 1 preparation.
Detailed description of the invention
In order to make the purpose of the present invention, technical scheme and advantage clearly understand, below in conjunction with drawings and Examples, the present invention is further elaborated.Should be appreciated that specific embodiment described herein is only in order to explain the present invention, is not intended to limit the present invention.
Described surname extraction is with dimethylbenzene, the organic solvent extraction cinnabar sample particles such as carbon tetrachloride, by controlling feeding quantity, organic solvent, extraction time, effectively to remove the elemental sulfur in root in Meng Usu, cinnabar micro-nano granules pattern after purification is preserved, purity is improved, and then the cinnabar micro-nano granules after purifying is distributed in the aqueous solution of polyvinylpyrrolidone (PVP), differential centrifugation is passed through after ultrasonic disperse, by controlling PVP concentration, rate of charge, centrifuge speed, centrifugation time can obtain the cinnabar micro-nano granules of different-grain diameter.
Embodiment 1
Step 1, the extraction of cinnabar sample particle:
Weigh 2g root in Meng Usu powder and wrap with filter paper, putting in apparatus,Soxhlet's.The dimethylbenzene of 150ml is placed in round-bottomed flask, at 150 DEG C, is heated backflow 6h, after natural cooling, described apparatus,Soxhlet's obtains cinnabar sample.Cinnabar sample is taken out, is positioned in fume hood 15h and the dimethylbenzene in cinnabar sample is volatilized, more described cinnabar sample is positioned in vacuum drying oven, at 50 DEG C, obtain cinnabar sample particle after dry 48 hours, be placed in drying baker standby.Sulfur free in sample is dissolved in dimethylbenzene, can obtain yellow sulfur crystal after decompression Distillation recovery dimethylbenzene.
Step 2, the differential of cinnabar micro-nano granules separates:
Step 2.1, weigh the cinnabar sample particle of 2g, described cinnabar sample particle is dispersed in PVP (polyvinylpyrrolidone) aqueous solution of 40mg/mL of 25ml, crosses Medium speed filter paper after ultrasonic disperse 30min, respectively obtain the cinnabar granule on filtrate and Medium speed filter paper；
Step 2.2, the cinnabar granule on described Medium speed filter paper, after deionized water and dehydrated alcohol wash 5 times respectively, is placed in vacuum drying oven, at 50 DEG C, dries and within 48 hours, obtains cinnabar 0# granule, and its particle diameter is more than 30 μm.
Step 2.3, proceed in the centrifuge tube of 10ml after described filtrate is stirred, after the centrifugal 5min of 1000rad/min, collect the suspension on described centrifuge tube top, described centrifuge tube adds the PVP aqueous solution of described same concentration, precipitation ultrasonic disperse bottom centrifuge tube is dissolved, continue with the centrifugal 5min of 1000rad/min, and the suspension on described centrifuge tube top is merged collection, repeatable operation 5 times, to described centrifuge tube top suspension clear, again by the precipitation bottom centrifuge tube after deionized water and dehydrated alcohol wash 5 times respectively, it is placed in vacuum drying oven, at 50 DEG C, dry and within 48 hours, obtain cinnabar 1# granule, its particle diameter is between 1-30 μm.
Step 2.4, proceeds in the centrifuge tube of 10ml by the suspension in step 2.3, repeats the operation of step 2.3, and centrifugal speed is brought up to 3000rad/min, obtain cinnabar 2# granule, and its particle diameter is between 0.2-1 μm.
Step 2.5, the suspension in step 2.4 proceeds in the centrifuge tube of 10ml, repeats the operation of step 2.3, and centrifugal speed is brought up to 5000rad/min, obtain cinnabar 3# granule, and its particle diameter is between 100-200nm.
Step 2.6, the suspension in step 2.5 proceeds in the centrifuge tube of 10ml, repeats the operation of step 2.3, and centrifugal speed is brought up to 7000rad/min, obtain cinnabar 4# granule, and its particle diameter is between 60-100nm.
Step 2.7, the suspension in step 2.6 proceeds in the centrifuge tube of 10ml, repeats the operation of step 2.3, and centrifugal speed is brought up to 9000rad/min, obtain cinnabar 5# granule, and its particle diameter is between 40-60nm.
Step 2.8, the suspension in step 2.7 proceeds in the centrifuge tube of 10ml, repeats the operation of step 2.3, and centrifugal speed is brought up to 11000rad/min, obtain cinnabar 6# granule, and its particle diameter is between 20-40nm.
Fig. 1 is electron scanning micrograph and the grain size distribution of the cinnabar micro-nano granules that embodiment 1 separates.It is irregular bulk that sample topography be can be observed, and each sample particle diameter is evenly distributed, and its grain size distribution shows in each sample that particle size distribution is close to normal distribution.A (), the SEM that (b) is 1# sample schemes and grain size distribution, between particle size range is 1-30 μm；C (), the SEM that (d) is 2# sample schemes and grain size distribution, between particle size range is 0.2-1 μm；E (), the SEM that (f) is 3# sample schemes and grain size distribution, and particle size range is between 100-200nm；G (), the SEM that (h) is 4# sample schemes and grain size distribution, and particle size range is between 60-100nm；I (), the SEM that (j) is 5# sample schemes and grain size distribution, and particle size range is between 40-60nm；K (), the SEM that (l) is 6# sample schemes and grain size distribution, and particle size range is between 20-40nm.
Fig. 2 is the XRD figure spectrum of the cinnabar nano-particle that embodiment 1 separates, and wherein abscissa is the angle of diffraction (2 θ), and unit is degree (deg.), and vertical coordinate is diffracted intensity, and unit is a.u..
Embodiment 2
Step 1, the extraction of cinnabar sample particle:
Weigh 1g root in Meng Usu powder and wrap with filter paper, putting in apparatus,Soxhlet's.The carbon tetrachloride of 100ml is placed in round-bottomed flask, at 100 DEG C, is heated backflow 4h, after natural cooling, described apparatus,Soxhlet's obtains cinnabar sample.Cinnabar sample is taken out, is positioned in fume hood 10h and the carbon tetrachloride in cinnabar sample is volatilized, more described cinnabar sample is positioned in vacuum drying oven, at 50 DEG C, obtain cinnabar sample particle after dry 48 hours, be placed in drying baker standby.Sulfur free in sample is dissolved in carbon tetrachloride, can obtain yellow sulfur crystal after decompression Distillation recovery carbon tetrachloride.
Step 2, the differential of cinnabar micro-nano granules separates:
Step 2.1, weighs the cinnabar sample particle of 1g, is dispersed in by described cinnabar sample particle in the PVP aqueous solution of 10mg/mL of 25ml, crosses Medium speed filter paper, respectively obtain the cinnabar granule on filtrate and Medium speed filter paper after ultrasonic disperse 30min；
Step 2.2, the cinnabar granule on described Medium speed filter paper, after deionized water and dehydrated alcohol wash 5 times respectively, is placed in vacuum drying oven, at 50 DEG C, dries and within 48 hours, obtains cinnabar 0# granule, and its particle diameter is more than 30 μm.
Step 2.3, proceed in the centrifuge tube of 10ml after described filtrate is stirred, after the centrifugal 3min of 1000rad/min, collect the suspension on described centrifuge tube top, described centrifuge tube adds the PVP aqueous solution of described same concentration, precipitation ultrasonic disperse bottom centrifuge tube is dissolved, continue with the centrifugal 3min of 1000rad/min, and the suspension on described centrifuge tube top is merged collection, repeatable operation 5 times, to described centrifuge tube top suspension clear, again by the precipitation bottom centrifuge tube after deionized water and dehydrated alcohol wash 5 times respectively, it is placed in vacuum drying oven, at 50 DEG C, dry and within 48 hours, obtain cinnabar 1# granule, its particle diameter is between 1-30 μm.
Step 2.4, proceeds in the centrifuge tube of 10ml by the suspension in step 2.3, repeats the operation of step 2.3, and centrifugal speed is brought up to 3000rad/min, obtain cinnabar 2# granule, and its particle diameter is between 0.2-1 μm.
Step 2.5, the suspension in step 2.4 proceeds in the centrifuge tube of 10ml, repeats the operation of step 2.3, and centrifugal speed is brought up to 5000rad/min, obtain cinnabar 3# granule, and its particle diameter is between 100-200nm.
Step 2.6, the suspension in step 2.5 proceeds in the centrifuge tube of 10ml, repeats the operation of step 2.3, and centrifugal speed is brought up to 7000rad/min, obtain cinnabar 4# granule, and its particle diameter is between 60-100nm.
Step 2.7, the suspension in step 2.6 proceeds in the centrifuge tube of 10ml, repeats the operation of step 2.3, and centrifugal speed is brought up to 9000rad/min, obtain cinnabar 5# granule, and its particle diameter is between 40-60nm.
Step 2.8, the suspension in step 2.7 proceeds in the centrifuge tube of 10ml, repeats the operation of step 2.3, and centrifugal speed is brought up to 11000rad/min, obtain cinnabar 6# granule, and its particle diameter is between 20-40nm.
Embodiment 3
Step 1, the extraction of cinnabar sample particle:
Weigh 3g root in Meng Usu powder and wrap with filter paper, putting in apparatus,Soxhlet's.The benzene of 180ml is placed in round-bottomed flask, at 120 DEG C, is heated backflow 8h, after natural cooling, described apparatus,Soxhlet's obtains cinnabar sample.Cinnabar sample is taken out, is positioned in fume hood 18h and the benzene in cinnabar sample is volatilized, more described cinnabar sample is positioned in vacuum drying oven, at 50 DEG C, obtain cinnabar sample particle after dry 48 hours, be placed in drying baker standby.Sulfur free in sample is dissolved in benzene, can obtain yellow sulfur crystal after decompression Distillation recovery benzene.
Step 2, the differential of cinnabar micro-nano granules separates:
Step 2.1, weighs the cinnabar sample particle of 3g, is dispersed in by described cinnabar sample particle in the PVP aqueous solution of 50mg/mL of 25ml, crosses Medium speed filter paper, respectively obtain the cinnabar granule on filtrate and Medium speed filter paper after ultrasonic disperse 30min；
Step 2.2, the cinnabar granule on described Medium speed filter paper, after deionized water and dehydrated alcohol wash 5 times respectively, is placed in vacuum drying oven, at 50 DEG C, dries and within 48 hours, obtains cinnabar 0# granule, and its particle diameter is more than 30 μm.
Step 2.3, proceed in the centrifuge tube of 10ml after described filtrate is stirred, after the centrifugal 6min of 1000rad/min, collect the suspension on described centrifuge tube top, described centrifuge tube adds the PVP aqueous solution of described same concentration, precipitation ultrasonic disperse bottom centrifuge tube is dissolved, continue with the centrifugal 5min of 1000rad/min, and the suspension on described centrifuge tube top is merged collection, repeatable operation 5 times, to described centrifuge tube top suspension clear, again by the precipitation bottom centrifuge tube after deionized water and dehydrated alcohol wash 5 times respectively, it is placed in vacuum drying oven, at 50 DEG C, dry and within 48 hours, obtain cinnabar 1# granule, its particle diameter is between 1-30 μm.
Step 2.4, proceeds in the centrifuge tube of 10ml by the suspension in step 2.3, repeats the operation of step 2.3, and centrifugal speed is brought up to 3000rad/min, obtain cinnabar 2# granule, and its particle diameter is between 0.2-1 μm.
Step 2.5, the suspension in step 2.4 proceeds in the centrifuge tube of 10ml, repeats the operation of step 2.3, and centrifugal speed is brought up to 5000rad/min, obtain cinnabar 3# granule, and its particle diameter is between 100-200nm.
Step 2.6, the suspension in step 2.5 proceeds in the centrifuge tube of 10ml, repeats the operation of step 2.3, and centrifugal speed is brought up to 7000rad/min, obtain cinnabar 4# granule, and its particle diameter is between 60-100nm.
Step 2.7, the suspension in step 2.6 proceeds in the centrifuge tube of 10ml, repeats the operation of step 2.3, and centrifugal speed is brought up to 9000rad/min, obtain cinnabar 5# granule, and its particle diameter is between 40-60nm.
Step 2.8, the suspension in step 2.7 proceeds in the centrifuge tube of 10ml, repeats the operation of step 2.3, and centrifugal speed is brought up to 11000rad/min, obtain cinnabar 6# granule, and its particle diameter is between 20-40nm.
Embodiment 4
Step 1, the extraction of cinnabar sample particle:
Weigh 4g root in Meng Usu powder and wrap with filter paper, putting in apparatus,Soxhlet's.The toluene of 200ml is placed in round-bottomed flask, at 120 DEG C, is heated backflow 10h, after natural cooling, described apparatus,Soxhlet's obtains cinnabar sample.Cinnabar sample is taken out, is positioned in fume hood 24h and the toluene in cinnabar sample is volatilized, more described cinnabar sample is positioned in vacuum drying oven, at 50 DEG C, obtain cinnabar sample particle after dry 48 hours, be placed in drying baker standby.Sulfur free in sample is dissolved in toluene, can obtain yellow sulfur crystal after decompression Distillation recovery toluene.
Step 2, the differential of cinnabar micro-nano granules separates:
Step 2.1, weighs the cinnabar sample particle of 2g, is dispersed in by described cinnabar sample particle in the PVP aqueous solution of 60mg/mL of 25ml, crosses Medium speed filter paper, respectively obtain the cinnabar granule on filtrate and Medium speed filter paper after ultrasonic disperse 30min；
Step 2.2, the cinnabar granule on described Medium speed filter paper, after deionized water and dehydrated alcohol wash 5 times respectively, is placed in vacuum drying oven, at 50 DEG C, dries and within 48 hours, obtains cinnabar 0# granule, and its particle diameter is more than 30 μm.
Step 2.3, proceed in the centrifuge tube of 10ml after described filtrate is stirred, after the centrifugal 6min of 1000rad/min, collect the suspension on described centrifuge tube top, described centrifuge tube adds the PVP aqueous solution of described same concentration, precipitation ultrasonic disperse bottom centrifuge tube is dissolved, continue with the centrifugal 5min of 1000rad/min, and the suspension on described centrifuge tube top is merged collection, repeatable operation 5 times, to described centrifuge tube top suspension clear, again by the precipitation bottom centrifuge tube after deionized water and dehydrated alcohol wash 5 times respectively, it is placed in vacuum drying oven, at 50 DEG C, dry and within 48 hours, obtain cinnabar 1# granule, its particle diameter is between 1-30 μm.
Step 2.4, proceeds in the centrifuge tube of 10ml by the suspension in step 2.3, repeats the operation of step 2.3, and centrifugal speed is brought up to 3000rad/min, obtain cinnabar 2# granule, and its particle diameter is between 0.2-1 μm.
Step 2.5, the suspension in step 2.4 proceeds in the centrifuge tube of 10ml, repeats the operation of step 2.3, and centrifugal speed is brought up to 5000rad/min, obtain cinnabar 3# granule, and its particle diameter is between 100-200nm.
Step 2.6, the suspension in step 2.5 proceeds in the centrifuge tube of 10ml, repeats the operation of step 2.3, and centrifugal speed is brought up to 7000rad/min, obtain cinnabar 4# granule, and its particle diameter is between 60-100nm.
Step 2.7, the suspension in step 2.6 proceeds in the centrifuge tube of 10ml, repeats the operation of step 2.3, and centrifugal speed is brought up to 9000rad/min, obtain cinnabar 5# granule, and its particle diameter is between 40-60nm.
Step 2.8, the suspension in step 2.7 proceeds in the centrifuge tube of 10ml, repeats the operation of step 2.3, and centrifugal speed is brought up to 11000rad/min, obtain cinnabar 6# granule, and its particle diameter is between 20-40nm.
Embodiment 5
Step 1, the extraction of cinnabar sample particle:
Weigh 5g root in Meng Usu powder and wrap with filter paper, putting in apparatus,Soxhlet's.The dimethylbenzene of 200ml is placed in round-bottomed flask, at 150 DEG C, is heated backflow 10h, after natural cooling, described apparatus,Soxhlet's obtains cinnabar sample.Cinnabar sample is taken out, is positioned in fume hood 20h and the dimethylbenzene in cinnabar sample is volatilized, more described cinnabar sample is positioned in vacuum drying oven, at 50 DEG C, obtain cinnabar sample particle after dry 48 hours, be placed in drying baker standby.Sulfur free in sample is dissolved in dimethylbenzene, can obtain yellow sulfur crystal after decompression Distillation recovery dimethylbenzene.
Step 2, the differential of cinnabar micro-nano granules separates:
Step 2.1, weighs the cinnabar sample particle of 5g, is dispersed in by described cinnabar sample particle in the PVP aqueous solution of 100mg/mL of 25ml, crosses Medium speed filter paper, respectively obtain the cinnabar granule on filtrate and Medium speed filter paper after ultrasonic disperse 30min；
Step 2.2, the cinnabar granule on described Medium speed filter paper, after deionized water and dehydrated alcohol wash 5 times respectively, is placed in vacuum drying oven, at 50 DEG C, dries and within 48 hours, obtains cinnabar 0# granule, and its particle diameter is more than 30 μm.
Step 2.3, proceed in the centrifuge tube of 10ml after described filtrate is stirred, after the centrifugal 10min of 1000rad/min, collect the suspension on described centrifuge tube top, described centrifuge tube adds the PVP aqueous solution of described same concentration, precipitation ultrasonic disperse bottom centrifuge tube is dissolved, continue with the centrifugal 5min of 1000rad/min, and the suspension on described centrifuge tube top is merged collection, repeatable operation 5 times, to described centrifuge tube top suspension clear, again by the precipitation bottom centrifuge tube after deionized water and dehydrated alcohol wash 5 times respectively, it is placed in vacuum drying oven, at 50 DEG C, dry and within 48 hours, obtain cinnabar 1# granule, its particle diameter is between 1-30 μm.
Step 2.4, proceeds in the centrifuge tube of 10ml by the suspension in step 2.3, repeats the operation of step 2.3, and centrifugal speed is brought up to 3000rad/min, obtain cinnabar 2# granule, and its particle diameter is between 0.2-1 μm.
Step 2.5, the suspension in step 2.4 proceeds in the centrifuge tube of 10ml, repeats the operation of step 2.3, and centrifugal speed is brought up to 5000rad/min, obtain cinnabar 3# granule, and its particle diameter is between 100-200nm.
Step 2.6, the suspension in step 2.5 proceeds in the centrifuge tube of 10ml, repeats the operation of step 2.3, and centrifugal speed is brought up to 7000rad/min, obtain cinnabar 4# granule, and its particle diameter is between 60-100nm.
Step 2.7, the suspension in step 2.6 proceeds in the centrifuge tube of 10ml, repeats the operation of step 2.3, and centrifugal speed is brought up to 9000rad/min, obtain cinnabar 5# granule, and its particle diameter is between 40-60nm.
Step 2.8, the suspension in step 2.7 proceeds in the centrifuge tube of 10ml, repeats the operation of step 2.3, and centrifugal speed is brought up to 11000rad/min, obtain cinnabar 6# granule, and its particle diameter is between 20-40nm.
Embodiment 6
Step 1, the extraction of cinnabar sample particle:
Weigh 5g root in Meng Usu powder and wrap with filter paper, putting in apparatus,Soxhlet's.The dimethylbenzene of 160ml is placed in round-bottomed flask, at 160 DEG C, is heated backflow 8h, after natural cooling, described apparatus,Soxhlet's obtains cinnabar sample.Cinnabar sample is taken out, is positioned in fume hood 16h and the dimethylbenzene in cinnabar sample is volatilized, more described cinnabar sample is positioned in vacuum drying oven, at 50 DEG C, obtain cinnabar sample particle after dry 48 hours, be placed in drying baker standby.Sulfur free in sample is dissolved in dimethylbenzene, can obtain yellow sulfur crystal after decompression Distillation recovery dimethylbenzene.
Step 2, the differential of cinnabar micro-nano granules separates:
Step 2.1, weighs the cinnabar sample particle of 4g, is dispersed in by described cinnabar sample particle in the PVP aqueous solution of 80mg/mL of 25ml, crosses Medium speed filter paper, respectively obtain the cinnabar granule on filtrate and Medium speed filter paper after ultrasonic disperse 30min；
Step 2.2, the cinnabar granule on described Medium speed filter paper, after deionized water and dehydrated alcohol wash 5 times respectively, is placed in vacuum drying oven, at 50 DEG C, dries and within 48 hours, obtains cinnabar 0# granule, and its particle diameter is more than 30 μm.
Step 2.3, proceed in the centrifuge tube of 10ml after described filtrate is stirred, after the centrifugal 7min of 1000rad/min, collect the suspension on described centrifuge tube top, described centrifuge tube adds the PVP aqueous solution of described same concentration, precipitation ultrasonic disperse bottom centrifuge tube is dissolved, continue with the centrifugal 5min of 1000rad/min, and the suspension on described centrifuge tube top is merged collection, repeatable operation 5 times, to described centrifuge tube top suspension clear, again by the precipitation bottom centrifuge tube after deionized water and dehydrated alcohol wash 5 times respectively, it is placed in vacuum drying oven, at 50 DEG C, dry and within 48 hours, obtain cinnabar 1# granule, its particle diameter is between 1-30 μm.
Step 2.4, proceeds in the centrifuge tube of 10ml by the suspension in step 2.3, repeats the operation of step 2.3, and centrifugal speed is brought up to 3000rad/min, obtain cinnabar 2# granule, and its particle diameter is between 0.2-1 μm.
Step 2.5, the suspension in step 2.4 proceeds in the centrifuge tube of 10ml, repeats the operation of step 2.3, and centrifugal speed is brought up to 5000rad/min, obtain cinnabar 3# granule, and its particle diameter is between 100-200nm.
Step 2.6, the suspension in step 2.5 proceeds in the centrifuge tube of 10ml, repeats the operation of step 2.3, and centrifugal speed is brought up to 7000rad/min, obtain cinnabar 4# granule, and its particle diameter is between 60-100nm.
Step 2.7, the suspension in step 2.6 proceeds in the centrifuge tube of 10ml, repeats the operation of step 2.3, and centrifugal speed is brought up to 9000rad/min, obtain cinnabar 5# granule, and its particle diameter is between 40-60nm.
Step 2.8, the suspension in step 2.7 proceeds in the centrifuge tube of 10ml, repeats the operation of step 2.3, and centrifugal speed is brought up to 11000rad/min, obtain cinnabar 6# granule, and its particle diameter is between 20-40nm.
The foregoing is only the preferred embodiments of the present invention, be not limited to the present invention, for a person skilled in the art, the present invention can have various modifications and variations.All within the spirit and principles in the present invention, any amendment of making, equivalent replacement, improvement etc., should be included within protection scope of the present invention.
Claims (9)
1. the extraction separation method of the cinnabar nano-particle in mongolian medicine root in Meng Usu, it is characterised in that comprise the following steps:
Step 1, the extraction of cinnabar sample particle:
Step 1.1, weighs 1-5g root in Meng Usu powder and wraps with filter paper, putting in apparatus,Soxhlet's；
Step 1.2, is placed in round-bottomed flask by the organic solvent of 100-200ml, is heated backflow 4-10h, obtains cinnabar sample in described apparatus,Soxhlet's at 100-160 DEG C；
Step 1.3, cinnabar sample is taken out, is positioned in fume hood 10-24h and the organic solvent in cinnabar sample is volatilized, more described cinnabar sample is positioned in vacuum drying oven, at 50 DEG C, it is placed in drying baker and obtains cinnabar sample particle after dry 48 hours；
Step 2, the differential of cinnabar micro-nano granules separates:
Step 2.1, weighs the cinnabar sample particle of 1-5g, is dispersed in by described cinnabar sample particle in the PVP solution of 10-100mg/mL of 25ml, crosses Medium speed filter paper, respectively obtain the cinnabar granule on filtrate and Medium speed filter paper after ultrasonic disperse 30min；
Step 2.2, the cinnabar granule on described Medium speed filter paper, after deionized water and dehydrated alcohol wash 5 times respectively, is placed in vacuum drying oven, at 50 DEG C, dries and within 48 hours, obtains cinnabar 0# granule；
Step 2.3, proceed in the centrifuge tube of 10ml after described filtrate is stirred, after the centrifugal 3-10min of 1000rad/min, collect the suspension on described centrifuge tube top, described centrifuge tube adds described PVP solution, precipitation ultrasonic disperse bottom centrifuge tube is dissolved, continue with the centrifugal 3-10min of 1000rad/min, and the suspension on described centrifuge tube top is merged collection, repeatable operation 3-5 time, again by the precipitation bottom centrifuge tube after deionized water and dehydrated alcohol wash 5 times respectively, it is placed in vacuum drying oven, at 50 DEG C, dry and within 48 hours, obtain cinnabar 1# granule；
Step 2.4, proceeds in the centrifuge tube of 10ml by the suspension in step 2.3, repeats the operation of step 2.3, and centrifugal speed is brought up to 3000rad/min, obtain cinnabar 2# granule；
Step 2.5, the suspension in step 2.4 proceeds in the centrifuge tube of 10ml, repeats the operation of step 2.3, and centrifugal speed is brought up to 5000rad/min, obtain cinnabar 3# granule；
Step 2.6, the suspension in step 2.5 proceeds in the centrifuge tube of 10ml, repeats the operation of step 2.3, and centrifugal speed is brought up to 7000rad/min, obtain cinnabar 4# granule；
Step 2.7, the suspension in step 2.6 proceeds in the centrifuge tube of 10ml, repeats the operation of step 2.3, and centrifugal speed is brought up to 9000rad/min, obtain cinnabar 5# granule；
Step 2.8, the suspension in step 2.7 proceeds in the centrifuge tube of 10ml, repeats the operation of step 2.3, and centrifugal speed is brought up to 11000rad/min, obtain cinnabar 6# granule；
Wherein, the cinnabar micro-nano granules of described cinnabar 0# granule, described cinnabar 1# granule, described cinnabar 2# granule, described cinnabar 3# granule, described cinnabar 4# granule, described cinnabar 5# granule, described cinnabar 6# granule respectively different-grain diameter.
2. the extraction separation method of the cinnabar nano-particle in mongolian medicine root in Meng Usu according to claim 1, it is characterised in that in step 1.1, weighs 2g root in Meng Usu powder.
3. the extraction separation method of the cinnabar nano-particle in mongolian medicine root in Meng Usu according to claim 1, it is characterised in that in step 1.2, described organic solvent is dimethylbenzene, carbon tetrachloride, benzene or toluene.
4. the extraction separation method of the cinnabar nano-particle in mongolian medicine root in Meng Usu according to claim 3, it is characterised in that described organic solvent is dimethylbenzene.
5. the extraction separation method of the cinnabar nano-particle in mongolian medicine root in Meng Usu according to claim 4, it is characterised in that in step 1.2, is heated backflow 4-10h at 150 DEG C.
6. the extraction separation method of the cinnabar nano-particle in mongolian medicine root in Meng Usu according to claim 1, it is characterised in that in step 2.1, weigh dried cinnabar sample in 2g step 1.3.
7. the extraction separation method of the cinnabar nano-particle in mongolian medicine root in Meng Usu according to claim 1, it is characterised in that described PVP solution concentration is 40mg/mL.
8. the extraction separation method of the cinnabar nano-particle in mongolian medicine root in Meng Usu according to claim 1, it is characterised in that in step 2.3, centrifugation time is 5min.
9. the extraction separation method of the cinnabar nano-particle in mongolian medicine root in Meng Usu according to claim 1, it is characterised in that described root in Meng Usu powder size is less than or equal to 200 orders.
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| CN110974846A (en) * | 2019-12-30 | 2020-04-10 | 内蒙古医科大学 | Method for separating nano-structure component from Mongolian medicine borneol and obtained nano-structure component |
| CN113304171A (en) * | 2021-05-26 | 2021-08-27 | 内蒙古医科大学 | Preparation method and application of targeted mercury sulfide nanoparticle medicine |
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| CN102633296A (en) * | 2012-05-04 | 2012-08-15 | 新疆大学 | Method for preparing mercuric sulfide (HgS) quantum dots by using mercury-containing wastewater |
| TW201236675A (en) * | 2011-03-02 | 2012-09-16 | Univ China Medical | Centrifugal purification/extraction method for effective composition of Chinese medicinal herb decoction |
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| CN1672720A (en) * | 2004-03-25 | 2005-09-28 | 香港理工大学 | Prepn process of Chinese medicine nano prepn |
| TW201236675A (en) * | 2011-03-02 | 2012-09-16 | Univ China Medical | Centrifugal purification/extraction method for effective composition of Chinese medicinal herb decoction |
| CN102633296A (en) * | 2012-05-04 | 2012-08-15 | 新疆大学 | Method for preparing mercuric sulfide (HgS) quantum dots by using mercury-containing wastewater |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110974846A (en) * | 2019-12-30 | 2020-04-10 | 内蒙古医科大学 | Method for separating nano-structure component from Mongolian medicine borneol and obtained nano-structure component |
| CN113304171A (en) * | 2021-05-26 | 2021-08-27 | 内蒙古医科大学 | Preparation method and application of targeted mercury sulfide nanoparticle medicine |
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