CN102564888A - Testing method for simultaneously determining volatile oil and impurity contents in frankincense or processed product thereof - Google Patents
Testing method for simultaneously determining volatile oil and impurity contents in frankincense or processed product thereof Download PDFInfo
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Abstract
The invention discloses a testing method for simultaneously determining volatile oil and impurity contents in frankincense or processed product thereof. The testing method includes the following steps: after the frankincense or the processed frankincense product is put into a round-bottomed flask and mixed with water, the round-bottomed flask is connected with a volatile oil measuring apparatus and a reflux condensing tube, the solution is slowly heated to boil, and is kept slightly boiling until the amount of oil in the measuring apparatus is not increased any more, heating is stopped, the solution is placed for a while, the valve of the lower end of the measuring apparatus is opened to slowly discharge water, and the volatile oil content is read; the solution and the undissolved part in the flask, which are still hot, are filtered by a gauze, the residue on the gauze is washed by hot water for three times, placed into the round-bottomed flask, added with solvent, heated, refluxed and filtered by a Buchner funnel before becoming cold, the flask is washed by solvent for three times, the residue is poured out onto the Buchner funnel and filtered, the residue on the Buchner funnel is transferred into a pre-constant-weight evaporating dish, the solvent is completely evaporated, and after low-temperature drying and weighing, the amount of impurities is obtained. The testing method can simultaneously determine volatile oil and impurity contents in the frankincense or the processed frankincense product, so that the active ingredients in the frankincense or the processed frankincense product cannot be destroyed.
Description
Technical field
The present invention relates to a kind of detection method, particularly relate to a kind of detection method of measuring volatile oil and impurity content in frankincense or the frankincense processed product simultaneously.
Background technology
Frankincense is the resin that olive subject plant Boswellia carterii Boswellia carterii Birdw. and congener Boswelliabhaw-dijiana Birdw. bark ooze out, and has the analgesic therapy of invigorating blood circulation, the effect of detumescence and promoting granulation.Under 207 pages of frankincense items of Pharmacopoeia of the People's Republic of China version in 2010, volatile oil contents assay method and limit standard have been stipulated.Different according to the source place, Somalia's frankincense contains volatile oil must not be less than 6.0% (ml/g), and Ethiopia's Olibanum volatile oil must not be less than 2.0% (ml/g).Stipulated the inspection method and the limit standard of impurity simultaneously, the frankincense pearl must not cross 2%, and former frankincense must not cross 10%.The inspection method of impurity in the Chinese medicine is to observe and impurity is picked with magnifier.And the impurity such as bark in the frankincense are mixed in frankincense, can't impurity directly be detected.If frankincense is smashed or pulverizes, the bark of the inside also powders simultaneously, and therefore, conventional Chinese medicine determination of foreign matter method also is not suitable for frankincense.There is bibliographical information to adopt the method for alkali treatment can measure the content of impurity in the frankincense, effectively, but also effective composition destroyed simultaneously.
Summary of the invention
The object of the present invention is to provide a kind of detection method of measuring volatile oil and impurity content in frankincense or the frankincense processed product simultaneously.
The present invention realizes through following technical scheme:
The present invention measures that the detection method of volatile oil and impurity content is in frankincense or the frankincense processed product: get frankincense or frankincense processed product 10-30 weight portion; The accurate title, decide, and puts in the round-bottomed flask, adds water 200-600 parts by volume; After jolting mixes; Connect volatile oil determination apparatus and reflux condensing tube, autocondensation pipe upper end adds water makes the scale part that is full of volatile oil determination apparatus, and overflow when going into flask till; Slowly be heated to and boil, and kept little 2-8 of boiling hour, oil mass no longer increases to the analyzer, stops heating, places a moment, opens the piston of analyzer lower end, and water is slowly emitted, and arrives to the oil reservoir upper end above scale 0 line till the 5mm place; Placed 0.5-2 hour, opening piston again, to make oil reservoir drop to its upper end just concordant with scale 0 line, reads the volatilization oil mass, and the number percent of volatile oil content in the calculating test sample; Solution filters with gauze with not dissolving part while hot in the flask, and residue is with hot wash 2-4 time on the gauze, and each 5-30 parts by volume is put gauze in the round-bottomed flask together with top residue then; Add solvent 20-300 parts by volume, ultrasonic or reflux 5-60 minute, filter with Buchner funnel while hot; Flask is with solvent wash 2-4 time, and each 5-30 parts by volume is poured on the Buchner funnel; Filter, residue is transferred in the evaporating dish of constant weight in advance on the Buchner funnel, volatilizes solvent; Low temperature drying 0.2-4.5 hour, claim that deciding weight is impurity level, calculates the number percent of impurity content.
The present invention measures simultaneously that the detection method of volatile oil and impurity content is preferably in frankincense or the frankincense processed product: get frankincense or frankincense processed product 20 weight portions; The accurate title, decide, and puts in the round-bottomed flask, adds water 300 parts by volume; After jolting mixes; Connect volatile oil determination apparatus and reflux condensing tube, autocondensation pipe upper end adds water makes the scale part that is full of volatile oil determination apparatus, and overflow when going into flask till; Slowly be heated to and boil, and keep little and boiled 6 hours, oil mass no longer increases to the analyzer, stops heating, places a moment, opens the piston of analyzer lower end, and water is slowly emitted, and arrives to the oil reservoir upper end above scale 0 line till the 5mm place; Placed 1 hour, opening piston again, to make oil reservoir drop to its upper end just concordant with scale 0 line, reads the volatilization oil mass, and the number percent of volatile oil content in the calculating test sample; Solution filters with gauze with not dissolving part while hot in the flask, and residue is with hot wash 3 times on the gauze, and each 10 parts by volume are put gauze in the round-bottomed flask together with top residue then; Add solvent 50 parts by volume, reflux 10 minutes filters with Buchner funnel while hot; Flask is with solvent wash 3 times, and each 10 parts by volume are poured on the Buchner funnel; Filter, residue is transferred in the evaporating dish of constant weight in advance on the Buchner funnel, volatilizes solvent; Low temperature drying 3 hours claims that deciding weight is impurity level, calculates the number percent of impurity content.
Solvent according to the invention is water and methyl alcohol, ethanol, normal butyl alcohol, acetone, ethyl acetate or ether.
The ratio of water according to the invention and methyl alcohol, ethanol, normal butyl alcohol, acetone, ethyl acetate or ether is 2-4: 5-9
The ratio of water according to the invention and methyl alcohol, ethanol, normal butyl alcohol, acetone, ethyl acetate or ether is 3: 7.
Solvent of the present invention also can be one or more of ethanol, methyl alcohol, acetone, ethyl acetate, ether, chloroform or sherwood oil.
Frankincense processed product according to the invention is stir-baked OLIBANUM, stir-baked OLIBANUM with vinegar, smoked frankincense or frankincense.
The corresponding relation of weight portion according to the invention and parts by volume is g/ml or kg/l.
The present invention can measure the content of frankincense or frankincense processed product (stir-baked OLIBANUM, stir-baked OLIBANUM with vinegar, smoked frankincense, frankincense) volatile oil contents and impurity simultaneously.Effective ingredient in frankincense or the frankincense processed product is not destroyed.
Test example below and be used to further specify the present invention, but be not limited to the present invention.
The assay method of volatile oil and impurity in experimental example frankincense or the frankincense processed product
Purpose: set up volatile oil and dirt content test method in frankincense or the frankincense processed product, foundation is provided for estimating frankincense or frankincense processed product quality.Method: investigated different solvents, compared ultrasonic, reflux two kinds of method for distilling, solvent load and extraction times.Result: contain water-soluble and liposoluble constituent in frankincense or the frankincense processed product, so can not use a kind of dissolution with solvents.Can add entry earlier and reflux, with water soluble ingredient dissolving and extraction volatile oil, add acetone or ethyl acetate or ethanol or aether backflow then, with the liposoluble constituent dissolving, remaining insolubles is impurity such as bark.Conclusion: this method can be used for the assay of volatile oil and impurity in frankincense or the frankincense processed product.
Frankincense is the resin that olive subject plant Boswellia carterii Boswellia carterii Birdw. and congener Boswelliabhaw-dijiana Birdw. bark ooze out, and has the analgesic therapy of invigorating blood circulation, the effect of detumescence and promoting granulation
[1]Under 207 pages of frankincense items of Pharmacopoeia of the People's Republic of China version in 2010, volatile oil contents assay method and limit standard have been stipulated.Different according to the source place, Somalia's frankincense or frankincense processed product contain volatile oil must not be less than 6.0% (ml/g), and Ethiopia's frankincense or frankincense processed product volatile oil must not be less than 2.0% (ml/g).Because commercially available frankincense or frankincense processed product all contain a certain amount of impurity, therefore, stipulate that former frankincense or frankincense processed product impurity must not surpass 10%, frankincense or frankincense processed product pearl must not cross 2%
[1]The inspection method of its impurity is to carry out according to the detection method of conventional Chinese medicine impurity; Promptly observe and impurity is picked fully with magnifier; And because the impurity in frankincense or the frankincense processed product is mixed in frankincense or the frankincense processed product is inner, only observes and can not impurity be picked fully with magnifier.The present invention is all dissolved frankincense or frankincense processed product when measuring the effective constituent volatile oil content, can obtain its whole impurity like this, to measure its impurity content.In the experiment extracting mode, solvent species and consumption, extraction time are investigated, optimized the method for frankincense or frankincense processed product impurity determination.Content to volatile oil and impurity in commercially available 11 batches of frankincenses or the frankincense processed product is measured, for the formulation of frankincense or frankincense processed product quality standard provides reference.
1, instrument, material and reagent
(1) instrument TCQ-250 ultrasonic cleaner (Beijing Medical Devices two factories); The OHAUS electronic balance; Temperature adjustable electrically heated cover; TAISITE electronic thermostatic water-bath; Volatilization has extraction apparatus (Beijing Glass Implement Factory).
(2) commercially available frankincense of material and reagent or frankincense processed product.Identify through the Liu Chunsheng professor of Beijing University of Chinese Medicine and to be the resin that olive subject plant Boswellia carterii Boswellia carterii Birdw. or congener Boswellia bhaw-dijianaBirdw. bark ooze out.Ethanol, methyl alcohol, normal butyl alcohol, acetone, ethyl acetate, ether, sherwood oil (analyze pure, Beijing Chemical Plant).
2, method and result
(1) solvent species is investigated
1) the single solvent reflow treatment is investigated
Get frankincense or frankincense processed product sample 5g, 9 parts, claim to decide weight, put in the triangular flask, add entry, ethanol, 70% ethanol, methyl alcohol, normal butyl alcohol, acetone, ethyl acetate, ether, sherwood oil 25mL respectively, water-bath reflux 2h.The result shows that all solvents all can not dissolve frankincense or processed product fully.The result shows, adopts the single solvent reflow treatment, can not be with the dissolving of all the components except that bark in frankincense or the frankincense processed product.
It should be noted that and adopt the water reflow treatment, remaining in the triangular flask is that impurity such as yellow insoluble matter and bark mix.And other solvent refluxing beyond the employing water is handled, and remaining in the triangular flask is that impurity such as white insoluble matter and bark mix.Explain that composition possibly be water-soluble part and the dissolution with solvents part of separating in frankincense or the frankincense processed product.If adopt two kinds of solvents reflow treatment successively, whole composition dissolvings that may impurity is outer.
2) two kinds of solvent reflow treatment investigations successively
If adopt water treatment earlier, can extract volatile oil and, adopt solvent processing then the water-soluble components dissolving, liposoluble constituent is dissolved.A kind of solvent in back more helps the drying of impurity such as bark.
Get frankincense or frankincense processed product sample 100g, claim to decide weight, put in the flask; Add entry 500mL refluxing extraction 2h, filter, solution filters with gauze with not dissolving part while hot in the flask; Residue is with hot wash 3 times on the gauze, and each 50mL is divided into several parts of about equivalent with the residue above the gauze then; Put respectively in the triangular flask, add ethanol, 70% ethanol, methyl alcohol, normal butyl alcohol, acetone, ethyl acetate, ether, sherwood oil 25mL, backflow or sonicated 30 minutes; The result shows; Can not be all the dissolving except that 70% ethanol and sherwood oil ultrasonic method with frankincense or frankincense processed product, other solvent adopts ultrasonic and reflow treatment, can be with frankincense or the outer whole compositions dissolvings of frankincense processed product impurity.
After showing employing water reflow treatment, select a kind of solvent to adopt reflow method or employing ultrasonic method (removing 70% ethanol, sherwood oil) again, can realize assay, and backflow is superior to ultrasonic impurity in frankincense or the frankincense processed product.The dissolution time of ethyl acetate and acetone is the shortest, is ethanol, methyl alcohol secondly, and 70% ethanol and sherwood oil are the slowest.
3) solvent load and return time
Get frankincense or the about 20g of frankincense processed product sample, 4 parts, claim to decide weight; Put respectively in the flask, add entry 300mL, connect volatile oil determination apparatus and reflux condensing tube; Slowly be heated to and boil, and keep little and boiled 6 hours, oil mass no longer increases to the analyzer; Placed 1 hour, and read the volatilization oil mass, calculate the number percent of volatile oil content in the test sample; Solution filters with gauze with not dissolving part while hot in the flask, and residue is with hot wash 3 times on the gauze, and each 20mL puts gauze in the round-bottomed flask together with top residue then; Add acetone 20ml respectively, 50ml, 100ml, 200ml; Reflux is observed the dissolving situation, the record dissolution time.The result shows that adding 20ml acetone reflux still had insolubles in 3 hours, adds reflux 10 minutes frankincenses or frankincense processed product of 50ml acetone and all dissolves, and drag only remains impurity such as bark.Add 100ml, 200ml and adding 50ml and do not have notable difference.
Show frankincense or frankincense processed product 20g, add the backflow of 50ml acetone and got final product in 10 minutes.
3, assay (according to embodiment 1 detection method): get frankincense or frankincense processed product 20g; The accurate title, decide, and puts in the round-bottomed flask, adds water 300ml; After jolting mixes; Connect volatile oil determination apparatus and reflux condensing tube, autocondensation pipe upper end adds water makes the scale part that is full of volatile oil determination apparatus, and overflow when going into flask till; Slowly be heated to and boil, and keep little and boiled 6 hours, oil mass no longer increases to the analyzer, stops heating, places a moment, opens the piston of analyzer lower end, and water is slowly emitted, and arrives to the oil reservoir upper end above scale 0 line till the 5mm place; Placed 1 hour, opening piston again, to make oil reservoir drop to its upper end just concordant with scale 0 line, reads the volatilization oil mass, and the number percent of volatile oil content in the calculating test sample; Solution filters with gauze with not dissolving part while hot in the flask, and residue is with hot wash 3 times on the gauze, and each 10ml puts gauze in the round-bottomed flask together with top residue then; Add acetone 50ml, reflux 10 minutes filters with Buchner funnel while hot; Flask is with washing with acetone 3 times, and each 10ml is poured on the Buchner funnel; Filter, residue is transferred in the evaporating dish of constant weight in advance on the Buchner funnel, volatilizes solvent; Low temperature drying 3 hours claims that deciding weight is impurity level, calculates the number percent of impurity content.The content results of volatile oil and impurity is seen table 1 in 11 batches of commercially available frankincenses measuring or the frankincense processed product.
The content of volatile oil and impurity in commercially available frankincense of table 1 or the frankincense processed product
4, discussion and conclusion
In the experiment assay method of volatile oil and impurity in frankincense or the frankincense processed product being investigated, is index with the dissolution degree of frankincense or frankincense processed product, has compared different single solvent reflow treatment, shows the detection of adopting a kind of solvent can not realize impurity.Through water and twice reflow treatment of other solvent priority, both can realize volatile oil contents mensuration, also can measure the content of impurity.And extract earlier volatile oil and dissolve water-soluble components with water, adopt solvent extraction then, can frankincense or frankincense processed product all be dissolved, and kept impurity such as bark.Selected solvent is best with acetoneand ethyl acetate, and backflow is superior to ultrasonic.When being solvent with acetone, solid-liquid ratio is 2: 5, and return time is 10 minutes.
Following embodiment is used to further specify the present invention, but is not limited to the present invention.
Embodiment
Embodiment 1:
Get frankincense 20g, accurate claim surely, put in the round-bottomed flask, add water 300ml, after jolting mixes, connect volatile oil determination apparatus and reflux condensing tube, autocondensation pipe upper end adds water makes the scale part that is full of volatile oil determination apparatus, and overflow when going into flask till; Slowly be heated to and boil, and keep little and boiled 6 hours, oil mass no longer increases to the analyzer, stops heating, places a moment, opens the piston of analyzer lower end, and water is slowly emitted, and arrives to the oil reservoir upper end above scale 0 line till the 5mm place; Placed 1 hour, opening piston again, to make oil reservoir drop to its upper end just concordant with scale 0 line, reads the volatilization oil mass, and the number percent of volatile oil content in the calculating test sample; Solution filters with gauze with not dissolving part while hot in the flask, and residue is with hot wash 3 times on the gauze, and each 10ml puts gauze in the round-bottomed flask together with top residue then; Add acetone 50ml, reflux 10 minutes filters with Buchner funnel while hot; Flask is with washing with acetone 3 times, and each 10ml is poured on the Buchner funnel; Filter, residue is transferred in the evaporating dish of constant weight in advance on the Buchner funnel, volatilizes solvent; Low temperature drying 3 hours claims that deciding weight is impurity level, calculates the number percent of impurity content.
Embodiment 2:
Get commercially available frankincense 20g (Chong Guang pharmaceutcal corporation, Ltd in Beijing produces-1), the accurate title, decide, and puts in the round-bottomed flask; After adding water 300ml jolting mixing; Connect volatile oil determination apparatus and reflux condensing tube, autocondensation pipe upper end adds water makes the scale part that is full of volatile oil determination apparatus, and overflow when going into flask till; Slowly be heated to and boil, and keep little and boiled 5 hours, oil mass no longer increases to the analyzer, stops heating, places a moment, opens the piston of analyzer lower end, and water is slowly emitted, and arrives to the oil reservoir upper end above scale 0 line till the 5mm place; Placed 0.8 hour, opening piston again, to make oil reservoir drop to its upper end just concordant with scale 0 line, read the volatilization oil mass, and volatile oil contents is 4.24% in the calculating test sample; Solution filters with gauze with not dissolving part while hot in the flask, and residue is with hot wash 3 times on the gauze, and each 10ml puts gauze in the round-bottomed flask together with top residue then; Add ethyl acetate 50ml, reflux 10 minutes filters with Buchner funnel while hot; Flask is with washing with alcohol 3 times, and each 5ml is poured on the Buchner funnel; Filter, residue is transferred in the evaporating dish of constant weight in advance on the Buchner funnel, volatilizes solvent; Low temperature drying 2 hours claims that deciding weight is impurity level, and the calculating impurity content is 2.4.%.
Embodiment 3:
Get commercially available frankincense 15g (Chinese traditional Chinese medical science institute clinic provide), accurately claim surely, put in the round-bottomed flask; Add water 500ml, after jolting mixes, connect volatile oil determination apparatus and reflux condensing tube; Autocondensation pipe upper end adds water makes the scale part that is full of volatile oil determination apparatus, and overflow when going into flask till; Slowly be heated to and boil, and keep little and boiled 3 hours, oil mass no longer increases to the analyzer, stops heating, places a moment, opens the piston of analyzer lower end, and water is slowly emitted, and arrives to the oil reservoir upper end above scale 0 line till the 5mm place; Placed 2 hours, opening piston again, to make oil reservoir drop to its upper end just concordant with scale 0 line, read the volatilization oil mass, and volatile oil content is 3.98% in the calculating test sample; Solution filters with gauze with not dissolving part while hot in the flask, and residue is with hot wash 2 times on the gauze, and each 20ml puts gauze in the round-bottomed flask together with top residue then; Add 70% ethanol 150ml, reflux 30 minutes filters with Buchner funnel while hot; Flask is with 70% washing with alcohol 2 times, and each 5ml is poured on the Buchner funnel; Filter, residue is transferred in the evaporating dish of constant weight in advance on the Buchner funnel, volatilizes solvent; Low temperature drying 0.5 hour claims that deciding weight is impurity level, and calculating impurity content is 0.75%.
Embodiment 4:
Get commercially available stir-baked OLIBANUM with vinegar 25g (production of doube bridge Beijing, Beijing prepared slices of Chinese crude drugs factory); The accurate title, decide, and puts in the round-bottomed flask, adds water 400ml; After jolting mixes; Connect volatile oil determination apparatus and reflux condensing tube, autocondensation pipe upper end adds water makes the scale part that is full of volatile oil determination apparatus, and overflow when going into flask till; Slowly be heated to and boil, and keep little and boiled 7 hours, oil mass no longer increases to the analyzer, stops heating, places a moment, opens the piston of analyzer lower end, and water is slowly emitted, and arrives to the oil reservoir upper end above scale 0 line till the 5mm place; Placed 2 hours, opening piston again, to make oil reservoir drop to its upper end just concordant with scale 0 line, read the volatilization oil mass, and volatile oil content is 1.78% in the calculating test sample; Solution filters with gauze with not dissolving part while hot in the flask, and residue is with hot wash 4 times on the gauze, and each 15ml puts gauze in the round-bottomed flask together with top residue then; Add ethanol and acetone (1: 1) mixed solvent 80ml, ultrasonic 12 minutes, filter with Buchner funnel while hot; Flask is with water washing 4 times, and each 15ml is poured on the Buchner funnel; Filter, residue is transferred in the evaporating dish of constant weight in advance on the Buchner funnel, volatilizes solvent; Low temperature drying 0.2 hour claims that deciding weight is impurity level, and calculating impurity content is 0.92%.
Embodiment 5:
Get stir-baked OLIBANUM 20g (the careless prepared slices of Chinese crude drugs in Beijing thousand factory provides), accurately claim surely, put in the round-bottomed flask; Add water 300ml, after jolting mixes, connect volatile oil determination apparatus and reflux condensing tube; Autocondensation pipe upper end adds water makes the scale part that is full of volatile oil determination apparatus, and overflow when going into flask till; Slowly be heated to and boil, and keep little and boiled 6 hours, oil mass no longer increases to the analyzer, stops heating, places a moment, opens the piston of analyzer lower end, and water is slowly emitted, and arrives to the oil reservoir upper end above scale 0 line till the 5mm place; Placed 0.6 hour, opening piston again, to make oil reservoir drop to its upper end just concordant with scale 0 line, read the volatilization oil mass, and volatile oil contents is 2.48% in the calculating test sample; Solution filters with gauze with not dissolving part while hot in the flask, and residue is with hot wash 3 times on the gauze, and each 10ml puts gauze in the round-bottomed flask together with top residue then; Add methyl alcohol 250ml, ultrasonic 16 minutes, filter with Buchner funnel while hot; Flask is with washing with acetone 3 times, and each 7ml is poured on the Buchner funnel; Filter, residue is transferred in the evaporating dish of constant weight in advance on the Buchner funnel, volatilizes solvent; Low temperature drying 3 hours claims that deciding weight is impurity level, and the content that calculates impurity is 1.3%.
Embodiment 6:
Get commercially available stir-baked OLIBANUM with vinegar 25g (medical insurance brand-new big pharmacy-1 in Beijing provides), the accurate title, decide, and puts in the round-bottomed flask; Add water 400ml, after jolting mixes, connect volatile oil determination apparatus and reflux condensing tube; Autocondensation pipe upper end adds water makes the scale part that is full of volatile oil determination apparatus, and overflow when going into flask till; Slowly be heated to and boil, and keep little and boiled 7 hours, oil mass no longer increases to the analyzer, stops heating, places a moment, opens the piston of analyzer lower end, and water is slowly emitted, and arrives to the oil reservoir upper end above scale 0 line till the 5mm place; Placed 1 hour, opening piston again, to make oil reservoir drop to its upper end just concordant with scale 0 line, read the volatilization oil mass, and volatile oil content is 2.04% in the calculating test sample; Solution filters with gauze with not dissolving part while hot in the flask, and residue is with hot wash 4 times on the gauze, and each 15ml puts gauze in the round-bottomed flask together with top residue then; Add EC (1: 1) mixed solvent 70ml, reflux 40 minutes filters with Buchner funnel while hot; Flask is with above-mentioned 70% washing with alcohol 2 times, and each 10ml is poured on the Buchner funnel; Filter, residue is transferred in the evaporating dish of constant weight in advance on the Buchner funnel, volatilizes solvent; Low temperature drying 4 hours claims that deciding weight is impurity level, and calculating impurity content is 2.2%.
Embodiment 7:
Get stir-baked OLIBANUM 20g (Beijing Jing Zhitang is big, and the pharmacy provides), the accurate title, decide, and puts in the round-bottomed flask; Add water 300ml, after jolting mixes, connect volatile oil determination apparatus and reflux condensing tube; Autocondensation pipe upper end adds water makes the scale part that is full of volatile oil determination apparatus, and overflow when going into flask till; Slowly be heated to and boil, and keep little and boiled 6 hours, oil mass no longer increases to the analyzer, stops heating, places a moment, opens the piston of analyzer lower end, and water is slowly emitted, and arrives to the oil reservoir upper end above scale 0 line till the 5mm place; Placed 1.2 hours, opening piston again, to make oil reservoir drop to its upper end just concordant with scale 0 line, read the volatilization oil mass, and volatile oil contents is 2.14% in the calculating test sample; Solution filters with gauze with not dissolving part while hot in the flask, and residue is with hot wash 3 times on the gauze, and each 5ml puts gauze in the round-bottomed flask together with top residue then; Add entry and acetone (3: 7) mixed solution 250ml, ultrasonic 16 minutes, filter with Buchner funnel while hot; Flask is with 70% methanol wash 3 times, and each 6ml is poured on the Buchner funnel; Filter, residue is transferred in the evaporating dish of constant weight in advance on the Buchner funnel, volatilizes solvent; Low temperature drying 0.6 hour claims that deciding weight is impurity level, and the content that calculates impurity is 3.8%.
Claims (10)
1. a detection method of measuring volatile oil and impurity content in frankincense or the frankincense processed product simultaneously is characterized in that this detection method is: get frankincense or frankincense processed product 10-30 weight portion; The accurate title, decide, and puts in the round-bottomed flask, adds water 200-600 parts by volume; After jolting mixes; Connect volatile oil determination apparatus and reflux condensing tube, autocondensation pipe upper end adds water makes the scale part that is full of volatile oil determination apparatus, and overflow when going into flask till; Slowly be heated to and boil, and kept little 2-8 of boiling hour, oil mass no longer increases to the analyzer, stops heating, places a moment, opens the piston of analyzer lower end, and water is slowly emitted, and arrives to the oil reservoir upper end above scale 0 line till the 5mm place; Placed 0.5-2 hour, opening piston again, to make oil reservoir drop to its upper end just concordant with scale 0 line, reads the volatilization oil mass, and the number percent of volatile oil content in the calculating test sample; Solution filters with gauze with not dissolving part while hot in the flask, and residue is with hot wash 2-4 time on the gauze, and each 5-30 parts by volume is put gauze in the round-bottomed flask together with top residue then; Add solvent 20-300 parts by volume, ultrasonic or reflux 5-60 minute, filter with Buchner funnel while hot; Flask is with solvent wash 2-4 time, and each 5-30 parts by volume is poured on the Buchner funnel; Filter, residue is transferred in the evaporating dish of constant weight in advance on the Buchner funnel, volatilizes solvent; Low temperature drying 0.2-4.5 hour, claim that deciding weight is impurity level, calculates the number percent of impurity content; The corresponding relation of said weight portion and parts by volume is g/ml or kg/l.
2. detection method as claimed in claim 1 is characterized in that, this detection method is: get frankincense or frankincense processed product 20 weight portions; The accurate title, decide, and puts in the round-bottomed flask, adds water 300 parts by volume; After jolting mixes; Connect volatile oil determination apparatus and reflux condensing tube, autocondensation pipe upper end adds water makes the scale part that is full of volatile oil determination apparatus, and overflow when going into flask till; Slowly be heated to and boil, and keep little and boiled 6 hours, oil mass no longer increases to the analyzer, stops heating, places a moment, opens the piston of analyzer lower end, and water is slowly emitted, and arrives to the oil reservoir upper end above scale 0 line till the 5mm place; Placed 1 hour, opening piston again, to make oil reservoir drop to its upper end just concordant with scale 0 line, reads the volatilization oil mass, and the number percent of volatile oil content in the calculating test sample; Solution filters with gauze with not dissolving part while hot in the flask, and residue is with hot wash 3 times on the gauze, and each 10 parts by volume are put gauze in the round-bottomed flask together with top residue then; Add solvent 50 parts by volume, ultrasonic or reflux 10 minutes filters with Buchner funnel while hot; Flask is with solvent wash 3 times, and each 10 parts by volume are poured on the Buchner funnel; Filter, residue is transferred in the evaporating dish of constant weight in advance on the Buchner funnel, volatilizes solvent; Low temperature drying 3 hours claims that deciding weight is impurity level, calculates the number percent of impurity content.
3. according to claim 1 or claim 2 detection method is characterized in that, said frankincense processed product is stir-baked OLIBANUM, stir-baked OLIBANUM with vinegar, smoked frankincense or frankincense.
4. according to claim 1 or claim 2 detection method is characterized in that said solvent is water and methyl alcohol, ethanol, normal butyl alcohol, acetone, ethyl acetate or ether.
5. according to claim 1 or claim 2 detection method is characterized in that said solvent is one or more of ethanol, methyl alcohol, acetone, ethyl acetate, ether, chloroform or sherwood oil.
6. detection method as claimed in claim 3 is characterized in that, said solvent is water and methyl alcohol, ethanol, normal butyl alcohol, acetone, ethyl acetate or ether.
7. detection method as claimed in claim 3 is characterized in that, said solvent is one or more of ethanol, methyl alcohol, acetone, ethyl acetate, ether, chloroform or sherwood oil.
8. detection method as claimed in claim 4 is characterized in that, the ratio of said water and methyl alcohol, ethanol, normal butyl alcohol, acetone, ethyl acetate or ether is 2-4: 5-9.
9. detection method as claimed in claim 6 is characterized in that, the ratio of said water and methyl alcohol, ethanol, normal butyl alcohol, acetone, ethyl acetate or ether is 2-4: 5-9.
10. like claim 8 or 9 described detection methods, it is characterized in that the ratio of said water and methyl alcohol, ethanol, normal butyl alcohol, acetone, ethyl acetate or ether is 3: 7.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114034600A (en) * | 2021-10-18 | 2022-02-11 | 柳州钢铁股份有限公司 | Method for measuring mechanical impurities of lubricating oil and direct-dropping type fat extractor |
| CN114748522A (en) * | 2022-05-26 | 2022-07-15 | 中国中医科学院中医基础理论研究所 | Boswellia carterii extract containing frankincense exosomes as well as preparation method and application thereof |
-
2010
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Non-Patent Citations (2)
| Title |
|---|
| 中国药典委员会: "《中国药典2005年版一部附录》", 31 December 2005 * |
| 贺拥军等: "《正交试验法优选乳香、没药等五味药挥发油的提取工艺》", 《陕西中医》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114034600A (en) * | 2021-10-18 | 2022-02-11 | 柳州钢铁股份有限公司 | Method for measuring mechanical impurities of lubricating oil and direct-dropping type fat extractor |
| CN114748522A (en) * | 2022-05-26 | 2022-07-15 | 中国中医科学院中医基础理论研究所 | Boswellia carterii extract containing frankincense exosomes as well as preparation method and application thereof |
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