CN103776930A - Cooling oil content measuring method - Google Patents
Cooling oil content measuring method Download PDFInfo
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- CN103776930A CN103776930A CN201410035390.6A CN201410035390A CN103776930A CN 103776930 A CN103776930 A CN 103776930A CN 201410035390 A CN201410035390 A CN 201410035390A CN 103776930 A CN103776930 A CN 103776930A
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Abstract
The invention discloses a cooling oil content measuring method. The cooling oil content measuring method comprises a step of qualitative and quantitative analysis on one or more ingredients of menthol, camphor, eucalyptol and eugenol. The method comprises the following specific steps: (1) taking the menthol, the camphor, the eucalyptol and the eugenol as reference objects; (2) treating a cooling oil sample by using a solvent, and then detecting the cooling oil sample by using a GC (Gas Chromatography) method; (3) a GC measuring method is as follows: a chromatographic column and a detector are used, wherein the chromatographic column is an HP-INNO WAX capillary column; the detector is a flame ionization detector; the temperature of the detector is 250-300 DEG C, the temperature of a sample inlet is 220-270 DEG C, the temperature of the column is increased in a programmed manner from an initial temperature of 60-110 DEG C to 220-280 DEG C, the temperature is increased by 5-15 DEG C every minute and kept for 8-20 minutes; sampling mode: split sampling is adopted, and the split ratio is 20:1. The method is scientific, reasonable, simple, convenient, easy to implement and suitable for quality control of volatile components including the menthol, the camphor and the like of the cooling oil and relevant extractives.
Description
Technical field
The present invention relates to the content assaying method of cooling ointment, be specifically related to the content assaying method of menthol, camphor, eucalyptol and eugenol in a kind of cooling ointment.
Background technology
The non-prescribed medicine that cooling ointment is made up of menthol, camphor, volatile oil extracted from eucalyptus' leaves or twigs, cloves wet goods raw material, has refrigerant heat radiation, arousing brain, raising spirit, and the merit of antipruritic pain relieving, is mainly used in cold headache, heatstroke, carsickness, mosquito bites and stings etc.Because drug effect is remarkable, and medicinal in extensive range and use till today, by consumers in general are favored.
At present, cooling ointment is domestic has 38 pharmaceutical manufacturers to produce this product, and authentication code has 41, also has in addition the refrigerant series products of adornment font size in market, and specification brand is all more.As the accurate font size of traditional Chinese medicines, the quality standard of cooling ointment is health Chinese medicine standard promulgated by the ministries or commissions of the Central Government (WS3-B-0144-89), and wherein mainly detecting index has discriminating, fusing point, assay, content uniformity, and wherein assay refers to detect wherein total volatile oil amount.Up to the present, have no the research report about Related Component in cooling ointment, without the assay method of menthol, camphor, eucalyptol and eugenol in this compound.
According to related requests such as traditional Chinese medicine quality standard method of analysis verification guide principles (one of Chinese Pharmacopoeia in 2010), set up the content assaying method (vapor-phase chromatography) of menthol in cooling ointment, camphor, eucalyptol and eugenol, carry out respectively methodological study, specifically comprised specificity test, serviceability test, linear relationship, precision test, stability test, detectability, replica test, average recovery test.Definite chromatographic condition is: chromatographic column: HP-INNOWAX capillary column (60m × 0.25mm, 0.25 μ m), detecting device: flame ionization ditector, detector temperature: 250-300 ℃, injector temperature: 220-270 ℃, column temperature: temperature programme, initial temperature 60-110 ℃, rises to 220-280 ℃, per minute 5-15 ℃, keep 8-20min, input mode: split sampling, split ratio 20:1.The method is scientific and reasonable, simple and easy to do, is applicable to the volatile ingredient such as menthol, camphor in cooling ointment and the quality control of associated extraction thing thereof.
Summary of the invention
The object of the invention is to, the content assaying method of volatility constituents in a kind of cooling ointment is provided, to overcome the existing above-mentioned shortcoming and defect of prior art.
The technical matters that will solve required for the present invention, can be achieved through the following technical solutions:
Cooling ointment content assaying method, is characterized in that, comprises the following steps:
(1) preparation of equipment and material
1. chromatographic condition
Chromatographic column: HP-INNOWAX capillary column, its specification is 60m × 0.25mm, 0.25 μ m, detecting device: flame ionization ditector, detector temperature: 250-300 ℃, injector temperature: 220-270 ℃, column temperature: temperature programme, initial temperature 60-110 ℃, rise to 220-280 ℃, per minute 5-15 ℃, keeps 8-20min, input mode: split sampling, split ratio 20:1.
2. the preparation of reference substance solution
It is appropriate, accurately weighed that precision takes menthol, camphor, eucalyptol and eugenol reference substance, and reagent adding is made respectively the mixing reference substance solution of every 1ml containing menthol 1.0-1.6mg, camphor 1.1-1.8mg, eucalyptol 0.8-1.2mg and eugenol 0.2-0.6mg.
3. the preparation of need testing solution
Get cooling ointment appropriate, mix, get 0.2g, accurately weighed, put in 25ml measuring bottle, add reagent 10ml, in 50 ℃ of water-baths, heat and within several minutes, make to melt, let cool, constant volume, shakes up, centrifugal, gets supernatant, to obtain final product.
(2) sample size is measured
Get respectively reference substance solution and need testing solution, inject gas chromatograph, records peak area, calculates respectively eucalyptol in cooling ointment, camphor, menthol and eugenol content by external standard method.
(3) methodological study project comprises: specificity test, serviceability test, linear relationship, precision test, stability test, detectability, replica test, average recovery test.
1. specificity test
According to above-mentioned chromatographic condition, draw reference substance solution, need testing solution and negative control solution, inject gas chromatograph respectively, number of theoretical plate calculates and is greater than 300000 by camphor, and degree of separation is all greater than 2; Show that component in negative control solution do not disturb the mensuration of corresponding reference substance.
2. serviceability test
It is HP-5MS capillary column that the present invention has investigated different chromatographic columns, fixing is (5%-phenyl)-methyl polysiloxane mutually, 0.25mm and 0.32mm, 0.25 μ m, 30m, and HP-INNOWAX capillary column, fixing is polyglycol (PEG) mutually, 60m × 0.25mm, 0.25 μ m, found that HP-INNOWAX capillary column is relatively applicable to the analyzing and testing of these 4 kinds of compositions;
In addition, parameter injector temperature, detector temperature, temperature programme speed, flow velocity are compared, find fine setting condition, the chromatographic peak theoretical cam curve of 4 kinds of compositions, degree of separation, tailing factor are all better.
3. linear relationship
Respectively by low concentration reference substance solution 1 μ l, middle concentration reference substance solution 1,2 μ l, high concentration reference substance solution inject gas chromatograph.
Measure by above-mentioned chromatographic condition, take the integrated value A of reference substance peak area as ordinate Y, sample size C(μ is g) horizontal ordinate X, carry out linear regression, obtaining regression equation is respectively: menthol A=690.09C+4.9889, r=0.9999(n=6), the range of linearity is 0.0286-2.86 μ g; Camphor A=673.90C+5.5854, r=0.9999(n=6), the range of linearity is 0.02852-2.852 μ g; Eucalyptol A=623.98C+3.6800, r=0.9999(n=6), the range of linearity is 0.0157842-1.57842 μ g; Eugenol A=624.76C+0.5610, r=0.9999(n=6), the range of linearity is 0.0043868-0.43868 μ g; Menthol, camphor, eucalyptol and eugenol are all good linear relationship in respective range.
4. precision test
Precision is got and is mixed reference substance solution 1 μ l, repeats sample introduction 6 times, records peak area and calculates relative standard deviation (RSD, %), and RSD is all less than 0.9%, shows that the precision of 4 kinds of compositions is all good;
5. stability test
4 kinds of reference substance solution RSD in 24h are all less than 2%, and stability is better.
6. detectability
Adopt signal to noise ratio (S/N ratio) method, get respectively appropriate menthol, camphor, eucalyptol and eugenol reference substance, accurately weighed, make highly concentrated solution by agent dissolves, concentration is respectively 0.3320mg/ml, 0.11682mg/ml, 0.52947mg/ml, 0.370884mg/ml; The lowest detectable limit concentration that obtains menthol, camphor, eucalyptol and eugenol reference substance is respectively 0.0006308mg/ml, 0.0005841mg/ml, 0.0052947mg/ml and 0.0029671mg/ml.
7. replica test
Get 6 parts, cooling ointment sample, by need testing solution, preparation method is prepared respectively, measure by sample determination method, and the equal <1% of average content RSD of 4 kinds of compositions, repeatability is better.
8. average recovery test
The cooling ointment sample of getting known content is appropriate, mix, get about 0.1g, 6 parts, accurately weighed, accurate eucalyptol, camphor, menthol and the eugenol reference substance adding with amount respectively, by need testing solution, preparation method prepares sample, calculate recovery rate, the average average recovery of menthol, camphor, eucalyptol and eugenol all meets the requirements, the equal <2% of RSD.
Further, the reagent that described reference substance solution and need testing solution preparation adopt refers to the one in 30-60 ℃ of sherwood oil, 60-90 ℃ sherwood oil, 90-120 ℃ sherwood oil, normal hexane, n-pentane and cyclohexane.
Further, also comprise the methodological study project of step (2) method of testing, comprising: specificity test, serviceability test, linear relationship, precision test, stability test, detectability, replica test, average recovery test.
Further, described specificity test: according to above-mentioned chromatographic condition, draw reference substance solution, need testing solution, negative control solution, inject gas chromatograph respectively, number of theoretical plate calculates and is greater than 300000 by camphor, and degree of separation is all greater than 2; Show that component in negative control solution do not disturb the mensuration of corresponding reference substance.
Further, described serviceability test: it is HP-5MS capillary column that different chromatographic columns have been investigated in test, fixing is (5%-phenyl)-methyl polysiloxane mutually, 0.25mm and 0.32mm, 0.25 μ m, 30m, with HP-INNOWAX capillary column, fixing is polyglycol (PEG) mutually, 60m × 0.25mm, 0.25 μ m, found that HP-INNOWAX capillary column is relatively applicable to the analyzing and testing of these 4 kinds of compositions; In addition, parameter injector temperature, detector temperature, temperature programme speed, flow velocity are compared, find fine setting condition, the chromatographic peak theoretical cam curve of 4 kinds of compositions, degree of separation, tailing factor are all better.
Further, described linear relationship: measure by above-mentioned chromatographic condition, take the integrated value A of reference substance peak area as ordinate Y, sample size C(μ is g) horizontal ordinate X, carry out linear regression, menthol, camphor, eucalyptol and eugenol are all good linear relationship in respective range.
Further, described precision test is all good.
Further, described stability test: 4 kinds of reference substance solution RSD in 24h are all less than 2%, and stability is better.
Further, described detectability: adopt signal to noise ratio (S/N ratio) method, obtain the lowest detectable limit concentration of menthol, camphor, eucalyptol and eugenol reference substance.
Further, described replica test: the equal <1% of average content RSD of 4 kinds of compositions, repeatability better.
Further, described average recovery test: the average average recovery of 4 kinds of compositions all meets the requirements, the equal <2% of RSD.
Beneficial effect of the present invention:
Cooling ointment content assaying method, has good accuracy, precision, specificity, detectability, the range of linearity, durability and stability.
Accompanying drawing explanation
Fig. 1 mixing reference substance collection of illustrative plates.
Fig. 2 negative control solution lacks the collection of illustrative plates of menthol.
Fig. 3 negative control solution lacks the collection of illustrative plates of camphor.
Fig. 4 negative control solution lacks the collection of illustrative plates of eucalyptol.
Fig. 5 negative control solution lacks the collection of illustrative plates of eugenol.
Fig. 6 need testing solution collection of illustrative plates.
Embodiment
Below in conjunction with specific embodiment, the invention will be further described.Should be understood that following examples are only for the present invention is described but not for limiting scope of the present invention.
Embodiment 1
Shown in specific as follows:
1 instrument material
7890A gas chromatograph (Agilent), 900B hydro-extractor (TOMOS), AB104-S analytical balance (METTLER TOLEDO)
Menthol reference substance (110728-200506, assay is used, National Institute for Food and Drugs Control), camphor reference substance (110747-201008, assay is used, content is in 99.0%, National Institute for Food and Drugs Control), eucalyptol reference substance (110788-201105, assay is used, content is in 99.9%, National Institute for Food and Drugs Control), eugenol reference substance (110725-201213, assay is used, content is in 99.7%, National Institute for Food and Drugs Control), 30-60 ℃ of sherwood oil, 60-90 ℃ of sherwood oil, 90-120 ℃ of sherwood oil, normal hexane, n-pentane and cyclohexane (are analysis pure, Shanghai Ling Feng chemical reagent company limited)
2 contents of the test
2.1 chromatographic condition
Chromatographic column: HP-INNOWAX capillary column (60m × 0.25mm, 0.25 μ m), detecting device: flame ionization ditector (FID), detector temperature: 250-300 ℃, injector temperature: 220-270 ℃, column temperature: temperature programme, initial temperature 60-110 ℃, rises to 220-280 ℃, per minute 5-15 ℃, keep 8-20min, input mode: split sampling, split ratio 20:1.
The preparation of 2.2 reference substance solution
It is appropriate, accurately weighed that precision takes menthol, camphor, eucalyptol and eugenol reference substance, and reagent adding is made respectively the mixing reference substance solution of every 1ml containing menthol 1.0-1.6mg, camphor 1.1-1.8mg, eucalyptol 0.8-1.2mg and eugenol 0.2-0.6mg.
The preparation of 2.3 need testing solutions
Get cooling ointment appropriate, mix, get 0.2g, accurately weighed, put in 25ml measuring bottle, add reagent 10ml, in 50 ℃ of water-baths, heat and within several minutes, make to melt, let cool, constant volume, shakes up, centrifugal, gets supernatant, to obtain final product.
2.4 sample sizes are measured
Accurate reference substance solution 1 μ l, the need testing solution 1 μ l of drawing respectively, inject gas chromatograph, records peak area, calculates respectively eucalyptol, camphor, menthol and eugenol content by external standard method, respectively cooling ointment product is measured, concrete content results sees the following form shown in 1.
Fig. 1 mixing reference substance collection of illustrative plates.Fig. 2 negative control solution lacks the collection of illustrative plates of menthol.Fig. 3 negative control solution lacks the collection of illustrative plates of camphor.Fig. 4 negative control solution lacks the collection of illustrative plates of eucalyptol.Fig. 5 negative control solution lacks the collection of illustrative plates of eugenol.Fig. 6 need testing solution collection of illustrative plates.Concrete collection of illustrative plates is as shown in Fig. 1-6.
The assay data of table 1 cooling ointment finished product
Above the specific embodiment of the present invention is illustrated, but the present invention is as limit, only otherwise depart from aim of the present invention, the present invention can also have various variations.
Claims (10)
1. a cooling ointment content assaying method, is characterized in that, comprises the following steps:
(1) preparation of equipment and material
1. chromatographic condition
Chromatographic column: HP-INNOWAX capillary column, its specification is 60m × 0.25mm, 0.25 μ m, detecting device: flame ionization ditector, detector temperature: 250-300 ℃, injector temperature: 220-270 ℃, column temperature: temperature programme, initial temperature 60-110 ℃, rises to 220-280 ℃, per minute 5-15 ℃, keep 8-20min, input mode: split sampling, split ratio 20:1;
2. the preparation of reference substance solution
It is appropriate, accurately weighed that precision takes menthol, camphor, eucalyptol and eugenol reference substance, and reagent adding is made respectively the mixing reference substance solution of every 1ml containing menthol 1.0-1.6mg, camphor 1.1-1.8mg, eucalyptol 0.8-1.2mg and eugenol 0.2-0.6mg;
3. the preparation of need testing solution
Get cooling ointment appropriate, mix, get 0.2g, accurately weighed, put in 25ml measuring bottle, add reagent 10ml, in 50 ℃ of water-baths, heat and within several minutes, make to melt, let cool, constant volume, shakes up, centrifugal, gets supernatant, to obtain final product;
(2) sample size is measured
Get respectively reference substance solution and need testing solution, inject gas chromatograph, records peak area, calculates respectively eucalyptol in cooling ointment, camphor, menthol and eugenol content by external standard method.
2. cooling ointment content assaying method according to claim 1, is characterized in that: the reagent that described reference substance solution and need testing solution preparation adopt refers to the one in 30-60 ℃ of sherwood oil, 60-90 ℃ sherwood oil, 90-120 ℃ sherwood oil, normal hexane, n-pentane and cyclohexane.
3. cooling ointment content assaying method according to claim 1, it is characterized in that: also comprise the methodological study project of step (2) method of testing, comprising: specificity test, serviceability test, linear relationship, precision test, stability test, detectability, replica test, average recovery test.
4. cooling ointment content assaying method according to claim 1, it is characterized in that: described specificity test: according to above-mentioned chromatographic condition, draw reference substance solution, need testing solution, negative control solution, inject gas chromatograph respectively, number of theoretical plate calculates and is greater than 300000 by camphor, and degree of separation is all greater than 2; Show that component in negative control solution do not disturb the mensuration of corresponding reference substance.
5. cooling ointment content assaying method according to claim 1, it is characterized in that: described serviceability test: it is HP-5MS capillary column that different chromatographic columns have been investigated in test, fixing is (5%-phenyl)-methyl polysiloxane mutually, 0.25mm and 0.32mm, 0.25 μ m, 30m, with HP-INNOWAX capillary column, fixing is polyglycol PEG mutually, 60m × 0.25mm, 0.25 μ m, found that HP-INNOWAX capillary column is relatively applicable to the analyzing and testing of these 4 kinds of compositions; In addition, parameter injector temperature, detector temperature, temperature programme speed, flow velocity are compared, find fine setting condition, the chromatographic peak theoretical cam curve of 4 kinds of compositions, degree of separation, tailing factor are all better.
6. cooling ointment content assaying method according to claim 1, it is characterized in that: described linear relationship: measure by above-mentioned chromatographic condition, take the integrated value A of reference substance peak area as ordinate Y, sample size C(μ is g) horizontal ordinate X, carry out linear regression, menthol, camphor, eucalyptol and eugenol are all good linear relationship in respective range.
7. cooling ointment content assaying method according to claim 1, is characterized in that: described stability test: 4 kinds of reference substance solution RSD in 24h are all less than 2%, and stability is better.
8. cooling ointment content assaying method according to claim 1, is characterized in that: described detectability: adopt signal to noise ratio (S/N ratio) method, obtain the lowest detectable limit concentration of menthol, camphor, eucalyptol and eugenol reference substance.
9. cooling ointment content assaying method according to claim 1, is characterized in that: described replica test: the equal <1% of average content RSD of 4 kinds of compositions, repeatability better.
10. cooling ointment content assaying method according to claim 1, is characterized in that: described average recovery test: the average average recovery of 4 kinds of compositions all meets the requirements, the equal <2% of RSD.
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Cited By (6)
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| CN104914194A (en) * | 2015-06-30 | 2015-09-16 | 四川新绿色药业科技发展股份有限公司 | Method for detecting menthol content of peppermint oil drop pill by gas chromatograph |
| CN105929050A (en) * | 2016-04-20 | 2016-09-07 | 广西壮族自治区梧州食品药品检验所 | Method for detecting content of eucalyptole in Folium Artemisiae Argyi |
| CN105954374A (en) * | 2016-04-20 | 2016-09-21 | 广西壮族自治区梧州食品药品检验所 | Method for determining content of eucalyptole in Folium Artemisiae Argyi by using gas chromatography |
| CN105954371A (en) * | 2016-04-20 | 2016-09-21 | 广西壮族自治区梧州食品药品检验所 | Method for determining content of eucalyptole in mouthwash by using gas chromatography |
| CN106018625A (en) * | 2016-07-21 | 2016-10-12 | 李时珍医药集团有限公司 | Method for detecting eucalyptol in moxa sticks |
| CN107748217A (en) * | 2017-10-20 | 2018-03-02 | 江苏康缘药业股份有限公司 | A kind of method for building up of Pisces particle GC quantitative finger print atlas and its application |
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Cited By (7)
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| CN104914194A (en) * | 2015-06-30 | 2015-09-16 | 四川新绿色药业科技发展股份有限公司 | Method for detecting menthol content of peppermint oil drop pill by gas chromatograph |
| CN104914194B (en) * | 2015-06-30 | 2019-11-29 | 四川新绿色药业科技发展有限公司 | A method of with Determination of menthol in gas chromatograph detection Dementholized mint oil dripping pill |
| CN105929050A (en) * | 2016-04-20 | 2016-09-07 | 广西壮族自治区梧州食品药品检验所 | Method for detecting content of eucalyptole in Folium Artemisiae Argyi |
| CN105954374A (en) * | 2016-04-20 | 2016-09-21 | 广西壮族自治区梧州食品药品检验所 | Method for determining content of eucalyptole in Folium Artemisiae Argyi by using gas chromatography |
| CN105954371A (en) * | 2016-04-20 | 2016-09-21 | 广西壮族自治区梧州食品药品检验所 | Method for determining content of eucalyptole in mouthwash by using gas chromatography |
| CN106018625A (en) * | 2016-07-21 | 2016-10-12 | 李时珍医药集团有限公司 | Method for detecting eucalyptol in moxa sticks |
| CN107748217A (en) * | 2017-10-20 | 2018-03-02 | 江苏康缘药业股份有限公司 | A kind of method for building up of Pisces particle GC quantitative finger print atlas and its application |
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