CN104297375B - The detection method of content of polyoxyethylene sorbitan monoleate in a kind of Chinese medicine 'Xuebijing ' injection - Google Patents
The detection method of content of polyoxyethylene sorbitan monoleate in a kind of Chinese medicine 'Xuebijing ' injection Download PDFInfo
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Abstract
The invention belongs to medical art, be specifically related to the gas-chromatography detection method of polyoxyethylene sorbitan monoleate in a kind of Chinese medicine 'Xuebijing ' injection.Detection method of the present invention, comprises the following steps: step 1, and prepared by reference substance solution: be reference substance with polyoxyethylene sorbitan monoleate, is mixed with reference substance solution; Step 2, the preparation of need testing solution: get 'Xuebijing ' injection and be mixed with need testing solution; Step 3, respectively by reference substance solution and need testing solution inject gas chromatograph, obtains chromatogram; Step 4, according to the chromatogram of chromatogram reference substance and test sample, through calculating the content of the polyoxyethylene sorbitan monoleate in need testing solution.
Description
Technical field
The invention belongs to medical art, be specifically related to the gas-chromatography detection method of polyoxyethylene sorbitan monoleate in a kind of Chinese medicine 'Xuebijing ' injection.
Background technology
'Xuebijing ' injection is through modern production process by Chinese crude drugs such as safflower, the radix paeoniae rubrathe, Ligusticum wallichii, the red sage root, Radix Angelicae Sinensis, and being aided with the modern Chinese herbal medicine preparation that suitable auxiliary material makes, the pharmacological property of its polycomponent, multipath, Mutiple Targets presents clear and definite curative effect in clinical treatment.
Polyoxyethylene sorbitan monoleate, has another name called: Tween 80 (Polysorbate80), for faint yellow to orange-yellow thick liquid; Micro-have special smell.Mildly bitter flavor is slightly puckery, has warmth sensation.Easily molten in water, ethanol, methyl alcohol or ethyl acetate, soluble,very slightly in mineral oil.The one of surfactant conventional in liquid preparation.For oil/water type emulsifying agent, can be used as stabilizing agent, diffusant, antistatic agent, fiber lubricant etc.React obtained by sorbitan monooleate and ethylene oxide.
'Xuebijing ' injection for increasing the surface tension of solution, increases the solubleness of medicine in preparation process, and the stability increasing solution adds a small amount of polyoxyethylene sorbitan monoleate.
At present, the parenteral solution containing polyoxyethylene sorbitan monoleate on market is a lot, but has certain spinoff because of polyoxyethylene sorbitan monoleate, therefore must be controlled its content, for this reason, researchist develops the detection method of polyoxyethylene sorbitan monoleate, as the method detected by HPLC ~ ELSD.ELSD is a kind of common detector, precision requirement relative average debiation≤5% of its testing result, and polyoxyethylene sorbitan monoleate is polyoxyethylene 2O sorbitol anhydride list oleic acid, and be a polymkeric substance, therefore the method precision is poor, and sensitivity is not strong, has certain limitation.
Chinese patent 201410140478.4 discloses the one method for quick of polyoxyethylene sorbitan monoleate " in the 'Xuebijing ' injection ", and the method adopts near infrared spectrum, is suitable for the Fast Measurement of tween ~ 80 content in 'Xuebijing ' injection.Can to on-line period such as the intermediate in 'Xuebijing ' injection production run, finished products, carry out the mensuration of tween ~ 80 at any time, to guarantee drug quality and production efficiency, testing cost is low, through reality compared with the conventional method, minute shortens dramatically, usual each sample completes within 1min, but because of as quick detection means, its accuracy of detection need to improve, therefore be only suitable for using in production run, be not suitable as sampling observation chemical examination use, be therefore necessary to find other method to detect for finished product outgoing quality.
Liposoluble constituent in tween ~ 80 and 'Xuebijing ' injection is as the parcel mutually such as forulic acid, tanshinone, senkyunolide I, and therefore separation difficulty, needs the separating agent finding matters.For this reason, the present invention has carried out sufficient research to related detection method, have found a kind of precision high, and simple to operate, applicability is strong.
Summary of the invention
The invention provides the gas-chromatography detection method of polyoxyethylene sorbitan monoleate in a kind of Chinese medicine 'Xuebijing ' injection.The vapor-phase chromatography that the present invention sets up detects the content of polyoxyethylene sorbitan monoleate in 'Xuebijing ' injection, compared with Evaporative light scattering detector (ELSD), the precision requirement relative average debiation of its testing result is≤2%, and comparatively ELSD detects and has greatly improved.
Cleaning Principle of the present invention is: the principal ingredient oleic acid in polyoxyethylene sorbitan monoleate is first free out through saponification, react with the methanol solution of boron trifluoride again and form methyl oleate, detect methyl oleate through vapor-phase chromatography, thus realize the quantitative detection to the polyoxyethylene sorbitan monoleate in Chinese medicine 'Xuebijing ' injection.Through Method validation, the content of polyoxyethylene sorbitan monoleate in 'Xuebijing ' injection can be detected by the method exactly, add the qualifying point of product, there is certain realistic meaning.Compared to additive method, method provided by the invention has the features such as specificity is strong, reproducible, sensitive, accurate.
For this reason, the invention provides the detection method of polyoxyethylene sorbitan monoleate in a kind of Chinese medicine 'Xuebijing ' injection, said method comprising the steps of:
Step 1, prepared by reference substance solution: take polyoxyethylene sorbitan monoleate as reference substance, be mixed with reference substance solution;
Step 2, the preparation of need testing solution: get 'Xuebijing ' injection and be mixed with need testing solution;
Step 3, respectively by reference substance solution and need testing solution inject gas chromatograph, obtains chromatogram;
Step 4, according to the chromatogram of chromatogram reference substance and test sample, through calculating the content of the polyoxyethylene sorbitan monoleate in need testing solution.
Wherein, the chromatographic condition of described gas chromatography is as follows:
Chromatographic column: HP ~ innowax (30m*0.32mm, 0.50um);
Injector temperature 260 ~ 280 DEG C;
Split ratio 1:50 ~ 70;
Detector temperature 300 ~ 360 DEG C;
Column temperature is 60 DEG C and keeps 0 minute, with the ramp to 160 DEG C of 20 DEG C per minute, keeps 1 minute, then with the ramp to 170 of 2 DEG C per minute DEG C ~ 190 DEG C, keeps 20 minutes;
Post flow is 1.0 ~ 3.0mL/min.
Theoretical half calculates should be not less than 10000 by methyl oleate peak.
Wherein, step 1, prepared by reference substance solution: method is as follows: take polyoxyethylene sorbitan monoleate 20 ~ 40mg, be placed in 40 ~ 60ml round-bottomed flask, add the methanol solution 1.5 ~ 2.5mL of 0.4 ~ 0.6mol/L NaOH, put in water-bath and add hot reflux 25 ~ 35min, let cool; Add the methanol solution 1.5 ~ 2.5mL of 12 ~ 16% boron trifluorides along condenser pipe, add hot reflux 25 ~ 35min, let cool; Along condenser pipe with normal heptane 3 ~ 5mL, continue backflow 8 ~ 12min, let cool; Extraction upper liquid, add saturated nacl aqueous solution 8 ~ 12mL, jolting 10 ~ 20 seconds, stratification, gets upper liquid, washes 1 ~ 3 time with water, each 3 ~ 5mL, and upper liquid, after anhydrous sodium sulfate drying, obtains reference substance solution.
Wherein, step 2, the preparation of need testing solution: method is as follows: precision measures 'Xuebijing ' injection 15 ~ 30ml, be placed in 40 ~ 60ml round-bottomed flask, be placed in evaporate to dryness in 80 DEG C ~ 100 DEG C water-baths, add the methanol solution 1.5 ~ 2.5mL of 0.4 ~ 0.6mol/L NaOH, put in water-bath and add hot reflux 25 ~ 35min, let cool; Add the methanol solution 1.5 ~ 2.5mL of 12 ~ 16% boron trifluorides along condenser pipe, add hot reflux 25 ~ 35min, let cool; Along condenser pipe with normal heptane 3 ~ 5mL, continue backflow 8 ~ 12min, let cool; Extraction upper liquid, add saturated nacl aqueous solution 8 ~ 12mL, jolting 10 ~ 20 seconds, stratification, gets upper liquid, washes 1 ~ 3 time with water, each 3 ~ 5mL, and upper liquid, after anhydrous sodium sulfate drying, obtains need testing solution.
Wherein, step 3, inject gas chromatograph: method is as follows: the above-mentioned reference substance solution of accurate absorption and each 0.8 ~ 1.2 μ l of need testing solution respectively, inject gas chromatograph, obtains chromatogram.
Preferably, method of the present invention, step is as follows:
Step 1, prepared by reference substance solution: method is as follows: precision takes polyoxyethylene sorbitan monoleate and is about 30mg, is placed in 50ml round-bottomed flask, adds the methanol solution 2mL of 0.5mol/L NaOH, puts in water-bath and add hot reflux 30min, let cool; Add the methanol solution 2mL of 14% boron trifluoride along condenser pipe, add hot reflux 30min, let cool; Along condenser pipe with normal heptane 4mL, continue backflow 10min, let cool; Extraction upper liquid, add saturated nacl aqueous solution 10mL, jolting 15 seconds, stratification, gets upper liquid, and wash with water 2 times (extraction), each 4mL, upper liquid, after anhydrous sodium sulfate drying, obtains reference substance solution.
Step 2, the preparation of need testing solution: method is as follows: precision measures 'Xuebijing ' injection 20ml, is placed in 50ml round-bottomed flask, be placed in evaporate to dryness in 100 DEG C of water-baths, add the methanol solution 2mL of 0.5mol/L NaOH, put in water-bath and add hot reflux 30min, let cool; Add the methanol solution 2mL of 14% boron trifluoride along condenser pipe, add hot reflux 30min, let cool; Along condenser pipe with normal heptane 4mL, continue backflow 10min, let cool; Extraction upper liquid, add saturated nacl aqueous solution 10mL, jolting 15 seconds, stratification, gets upper liquid, and wash with water 2 times (extraction), each 4mL, upper liquid, after anhydrous sodium sulfate drying, obtains need testing solution.
Step 3, inject gas chromatograph: method is as follows: the above-mentioned reference substance solution of accurate absorption and each 1 μ l of need testing solution respectively, inject gas chromatograph, obtains chromatogram.
The compound method etc. of chromatographic condition of the present invention and solution is through inventor and screens rear acquisition, and screening process is as follows:
1, injector temperature
The temperature of injection port is screened, to investigate injector temperature to the impact detected.The results are shown in Table 1.
'Xuebijing ' injection testing result under the different injector temperature of table 1
| Injector temperature (DEG C) | 250 | 260 | 270 | 280 | 290 |
| Tailing factor | 0.904 | 0.981 | 0.985 | 0.970 | 0.940 |
| Peak height | 23284.2 | 38258.1 | 38245.4 | 39041.6 | 39897.7 |
From upper table result we think: tailing factor should control between 1.05 ~ 095, peak height more than 35000 is better, and therefore injector temperature controls within the scope of 260 DEG C ~ 280 DEG C.
2, split ratio
Split ratio is screened, to investigate the impact of shunting Determination.The results are shown in Table 2.
'Xuebijing ' injection testing result under the different split ratio of table 2
| Split ratio | 1:40 | 1:50 | 1:60 | 1:70 | 1:80 |
| Peak area | 104335.6 | 71675.4 | 650659.2 | 577842.5 | 454662.3 |
From upper table result we think: peak area to control between 50000 ~ 80000 better, and therefore split ratio controls within the scope of 1:50 ~ 1:70.
3, detector temperature
The temperature of detecting device is screened, to investigate detector temperature to the impact detected.The results are shown in Table 3.
'Xuebijing ' injection testing result under the different detector temperature of table 3
| Detector temperature (DEG C) | 280 | 300 | 330 | 360 | 390 |
| Theoretical tray | 20451.692 | 46781.411 | 50482.365 | 48351.587 | 30154.940 |
From upper table result we think: theoretical cam curve controls be greater than 45000 better, and therefore detector temperature controls within the scope of 300 DEG C ~ 360 DEG C.
4, column temperature
The change of column temperature can change peak shape and the peak width of chromatographic peak, therefore screens the heating schedule of gas chromatographic column column oven, to investigate column temperature to the impact detected.The results are shown in Table 4.
'Xuebijing ' injection testing result under the different column temperature of table 4
| Final column temperature (DEG C) | 160 | 170 | 180 | 190 | 200 |
| Theoretical tray | 26011.048 | 45276.234 | 49880.520 | 47154.329 | 223392.18 |
From upper table result we think: theoretical cam curve controls be greater than 45000 better, and therefore final column temperature controls within the scope of 170 DEG C ~ 190 DEG C.
5, post flow
Coupled columns flow is explored, to investigate post flow to the impact detected.The results are shown in Table 5.
'Xuebijing ' injection testing result under the different post flow of table 5
| Post flow (ml/min) | 0.5 | 1.0 | 2.0 | 3.0 | 4.0 |
| Appearance time (min) | 38.245 | 33.326 | 26.181 | 22.796 | 12.334 |
From upper table result we think: appearance time controls at 20 ~ 35min better, and therefore post flow is good at 1.0 ~ 3.0ml/min.
6, liquid evaporate to dryness (water-bath) temperature
Sample evaporate to dryness temperature is screened, to investigate evaporate to dryness temperature to the impact detected.The results are shown in Table 6.
'Xuebijing ' injection testing result under the different bath temperature of table 6
| Temperature (DEG C) | 70 | 80 | 90 | 100 |
| Peak area | 24335.6 | 65675.4 | 650659.2 | 677842.5 |
| Required time | About 8h | About 4h | About 3.5h | About 2h |
From upper table result we think: under 70 DEG C of water-baths, evaporate to dryness liquid required time is longer; And the esterification effect of sample can be affected, cause peak area compared with normal little.Therefore liquid evaporate to dryness (water-bath) temperature controls within the scope of 80 DEG C ~ 100 DEG C.
Detection method of the present invention, has the following advantages:
The off-line quality control of product: the qualifying point adding product, can in storage period, transport and clinical practice in 'Xuebijing ' injection carry out quality control.
The present invention, relative to prior art, mainly to the precision that improve detection method, is more applicable for the offline inspection of product.
Get a collection of Chinese medicine 'Xuebijing ' injection, measure by condition of the present invention, parallel 6 increment product, continuous sample introduction 2 times, calculate RSD% (≤2%).
Embodiment
Embodiment is only described further summary of the invention, is not limited to embodiment content.
Embodiment 1:
Chromatographic condition chromatographic column: HP ~ innowax (30m*0.32mm, 0.50um); Injector temperature 270 DEG C, split ratio 1:60, detector temperature 330 DEG C, column temperature is 60 DEG C and keeps 0 minute, with the ramp to 160 DEG C of 20 DEG C per minute, keeps 1 minute, then with the ramp to 180 DEG C of 2 DEG C per minute, keeps 20 minutes; Post flow is 3.0mL/min.Theoretical half calculates should be not less than 10000 by methyl oleate peak.
Sample prepare sample thief, be placed in 50ml round-bottomed flask, add the methanol solution 2mL of 0.5mol/L NaOH, put in water-bath and add hot reflux 30min, let cool; Add the methanol solution 2mL of 14% boron trifluoride along condenser pipe, add hot reflux 30min, let cool; Along condenser pipe with normal heptane 4mL, continue backflow 10min, let cool; Extraction upper liquid, add saturated nacl aqueous solution 10mL, jolting 15 seconds, stratification, gets upper liquid, and wash with water 2 times (extraction), each 4mL, upper liquid, after anhydrous sodium sulfate drying, enters gas chromatographic detection.
Reference substance solution is prepared precision and is taken polyoxyethylene sorbitan monoleate and be about 30mg, prepares reference substance solution according under " preparation of sample " item.
The preparation precision of need testing solution measures 'Xuebijing ' injection 20ml, is placed in 50ml round-bottomed flask, is positioned on 100 DEG C of water-baths and heats evaporate to dryness, prepares sample solution according under " preparation of sample " item.
Determination method is accurate respectively draws above-mentioned reference substance solution and each 1 μ l of need testing solution, inject gas chromatograph, measures, to obtain final product.
Embodiment 2
Chromatographic condition chromatographic column: HP ~ innowax (30m*0.32mm, 0.50um); Injector temperature 270 DEG C, split ratio 1:50, detector temperature 330 DEG C, column temperature is 60 DEG C and keeps 0 minute, with the ramp to 160 DEG C of 20 DEG C per minute, keeps 1 minute, then with the ramp to 200 DEG C of 2 DEG C per minute, keeps 20 minutes; Post flow is 2.0mL/min.Theoretical half calculates should be not less than 10000 by methyl oleate peak.
Sample prepare sample thief, be placed in 50ml round-bottomed flask, add the methanol solution 2mL of 0.5mol/L NaOH, put in water-bath and add hot reflux 30min, let cool; Add the methanol solution 2mL of 14% boron trifluoride along condenser pipe, add hot reflux 30min, let cool; Along condenser pipe with normal heptane 4mL, continue backflow 10min, let cool; Extraction upper liquid, add saturated nacl aqueous solution 10mL, jolting 15 seconds, stratification, gets upper liquid, and wash with water 2 times (extraction), each 4mL, upper liquid, after anhydrous sodium sulfate drying, enters gas chromatographic detection.
Reference substance solution is prepared precision and is taken polyoxyethylene sorbitan monoleate and be about 30mg, prepares reference substance solution according under " preparation of sample " item.
The preparation precision of need testing solution measures 'Xuebijing ' injection 20ml, is placed in 50ml round-bottomed flask, is positioned on 90 DEG C of water-baths and heats evaporate to dryness, prepares sample solution according under " preparation of sample " item.
Determination method is accurate respectively draws above-mentioned reference substance solution and each 1 μ l of need testing solution, inject gas chromatograph, measures, to obtain final product.
Embodiment 3
Chromatographic condition chromatographic column: HP ~ innowax (30m*0.32mm, 0.50um); Injector temperature 270 DEG C, split ratio 1:80, detector temperature 330 DEG C, column temperature is 60 DEG C and keeps 0 minute, with the ramp to 220 DEG C of 20 DEG C per minute, keeps 1 minute, then with the ramp to 220 DEG C of 2 DEG C per minute, keeps 20 minutes; Post flow is 1.0mL/min.Theoretical half calculates should be not less than 10000 by methyl oleate peak.
Sample prepare sample thief, be placed in 50ml round-bottomed flask, add the methanol solution 2mL of 0.5mol/L NaOH, put in water-bath and add hot reflux 30min, let cool; Add the methanol solution 2mL of 14% boron trifluoride along condenser pipe, add hot reflux 30min, let cool; Along condenser pipe with normal heptane 4mL, continue backflow 10min, let cool; Extraction upper liquid, add saturated nacl aqueous solution 10mL, jolting 15 seconds, stratification, gets upper liquid, and wash with water 2 times (extraction), each 4mL, upper liquid, after anhydrous sodium sulfate drying, enters gas chromatographic detection.
Reference substance solution is prepared precision and is taken polyoxyethylene sorbitan monoleate and be about 30mg, prepares reference substance solution according under " preparation of sample " item.
The preparation precision of need testing solution measures 'Xuebijing ' injection 20ml, is placed in 50ml round-bottomed flask, is positioned on 80 DEG C of water-baths and heats evaporate to dryness, prepares sample solution according under " preparation of sample " item.
Determination method is accurate respectively draws above-mentioned reference substance solution and each 1 μ l of need testing solution, inject gas chromatograph, measures, to obtain final product.
Claims (8)
1. the detection method of content of polyoxyethylene sorbitan monoleate in Chinese medicine 'Xuebijing ' injection, is characterized in that, said method comprising the steps of:
Step 1, prepared by reference substance solution: take polyoxyethylene sorbitan monoleate as reference substance, be mixed with reference substance solution;
Step 2, the preparation of need testing solution: get 'Xuebijing ' injection and be mixed with need testing solution;
Step 3, respectively by reference substance solution and need testing solution inject gas chromatograph, obtains chromatogram;
Step 4, according to the chromatogram of reference substance and test sample, through calculating the content of the polyoxyethylene sorbitan monoleate in need testing solution;
Wherein, the chromatographic condition of described gas chromatography is as follows:
Chromatographic column: HP ~ innowax, model 30m × 0.32mm, 0.50 μm;
Injector temperature 260 ~ 280 DEG C,
Split ratio 1:50 ~ 70,
Detector temperature 300 ~ 360 DEG C,
Column temperature is 60 DEG C and keeps 0 minute, with the ramp to 160 DEG C of 20 DEG C per minute, keeps 1 minute, then with the ramp to 170 of 2 DEG C per minute DEG C ~ 190 DEG C, keeps 20 minutes;
Post flow is 1.0 ~ 3.0mL/min.
2. detection method according to claim 1, it is characterized in that, wherein, step 1, prepared by reference substance solution: method is as follows: take polyoxyethylene sorbitan monoleate 20 ~ 40mg, is placed in 40 ~ 60ml round-bottomed flask, adds the methanol solution 1.5 ~ 2.5mL of 0.4 ~ 0.6mol/L NaOH, put in water-bath and add hot reflux 25 ~ 35min, let cool; Add the methanol solution 1.5 ~ 2.5mL of 14% boron trifluoride along condenser pipe, add hot reflux 25 ~ 35min, let cool; Along condenser pipe with normal heptane 3 ~ 5mL, continue backflow 8 ~ 12min, let cool; Extraction upper liquid, add saturated nacl aqueous solution 8 ~ 12mL, jolting 10 ~ 20 seconds, stratification, gets upper liquid, washes 1 ~ 3 time with water, each 3 ~ 5mL, and upper liquid, after anhydrous sodium sulfate drying, obtains reference substance solution.
3. detection method according to claim 1, it is characterized in that, wherein, step 2, the preparation of need testing solution: method is as follows: precision measures 'Xuebijing ' injection 15 ~ 30ml, is placed in 40 ~ 60ml round-bottomed flask, be placed in evaporate to dryness in 80 DEG C ~ 100 DEG C water-baths, add the methanol solution 1.5 ~ 2.5mL of 0.4 ~ 0.6mol/L NaOH, put in water-bath and add hot reflux 25 ~ 35min, let cool; Add the methanol solution 1.5 ~ 2.5mL of 14% boron trifluoride along condenser pipe, add hot reflux 25 ~ 35min, let cool; Along condenser pipe with normal heptane 3 ~ 5mL, continue backflow 8 ~ 12min, let cool; Extraction upper liquid, add saturated nacl aqueous solution 8 ~ 12mL, jolting 10 ~ 20 seconds, stratification, gets upper liquid, washes 1 ~ 3 time with water, each 3 ~ 5mL, and upper liquid, after anhydrous sodium sulfate drying, obtains need testing solution.
4. detection method according to claim 1, it is characterized in that, wherein, inject gas chromatograph described in step 3: method is as follows: the above-mentioned reference substance solution of accurate absorption and each 0.8 ~ 1.2 μ l of need testing solution respectively, inject gas chromatograph, obtains chromatogram.
5. detection method according to claim 1, is characterized in that, step 1, prepared by reference substance solution: method is as follows: precision takes polyoxyethylene sorbitan monoleate and is about 30mg, is placed in 50ml round-bottomed flask, adds the methanol solution 2mL of 0.5mol/L NaOH, put in water-bath and add hot reflux 30min, let cool; Add the methanol solution 2mL of 14% boron trifluoride along condenser pipe, add hot reflux 30min, let cool; Along condenser pipe with normal heptane 4mL, continue backflow 10min, let cool; Extraction upper liquid, add saturated nacl aqueous solution 10mL, jolting 15 seconds, stratification, gets upper liquid, washes 2 times with water, each 4mL, and upper liquid, after anhydrous sodium sulfate drying, obtains reference substance solution.
6. detection method according to claim 1, it is characterized in that, step 2, the preparation of need testing solution: method is as follows: precision measures 'Xuebijing ' injection 20ml, be placed in 50ml round-bottomed flask, be placed in evaporate to dryness in 100 DEG C of water-baths, add the methanol solution 2mL of 0.5mol/L NaOH, put in water-bath and add hot reflux 30min, let cool; Add the methanol solution 2mL of 14% boron trifluoride along condenser pipe, add hot reflux 30min, let cool; Along condenser pipe with normal heptane 4mL, continue backflow 10min, let cool; Extraction upper liquid, add saturated nacl aqueous solution 10mL, jolting 15 seconds, stratification, gets upper liquid, washes 2 times with water, each 4mL, and upper liquid, after anhydrous sodium sulfate drying, obtains need testing solution.
7. detection method according to claim 1, is characterized in that, inject gas chromatograph described in step 3: method is as follows: the above-mentioned reference substance solution of accurate absorption and each 1 μ l of need testing solution respectively, inject gas chromatograph, obtains chromatogram.
8. detection method according to claim 1, is characterized in that, step is as follows:
Step 1, prepared by reference substance solution: method is as follows: precision takes polyoxyethylene sorbitan monoleate and is about 30mg, is placed in 50ml round-bottomed flask, adds the methanol solution 2mL of 0.5mol/L NaOH, puts in water-bath and add hot reflux 30min, let cool; Add the methanol solution 2mL of 14% boron trifluoride along condenser pipe, add hot reflux 30min, let cool; Along condenser pipe with normal heptane 4mL, continue backflow 10min, let cool; Extraction upper liquid, add saturated nacl aqueous solution 10mL, jolting 15 seconds, stratification, gets upper liquid, washes 2 times with water, each 4mL, and upper liquid, after anhydrous sodium sulfate drying, obtains reference substance solution;
Step 2, the preparation of need testing solution: method is as follows: precision measures 'Xuebijing ' injection 20ml, is placed in 50ml round-bottomed flask, be placed in evaporate to dryness in 100 DEG C of water-baths, add the methanol solution 2mL of 0.5mol/L NaOH, put in water-bath and add hot reflux 30min, let cool; Add the methanol solution 2mL of 14% boron trifluoride along condenser pipe, add hot reflux 30min, let cool; Along condenser pipe with normal heptane 4mL, continue backflow 10min, let cool; Extraction upper liquid, add saturated nacl aqueous solution 10mL, jolting 15 seconds, stratification, gets upper liquid, washes 2 times with water, each 4mL, and upper liquid, after anhydrous sodium sulfate drying, obtains need testing solution;
Step 3, described inject gas chromatograph: method is as follows: the above-mentioned reference substance solution of accurate absorption and each 1 μ l of need testing solution respectively, inject gas chromatograph, obtains chromatogram;
Step 4, according to the chromatogram of reference substance and test sample, through calculating the content of the polyoxyethylene sorbitan monoleate in need testing solution;
Chromatographic condition
Chromatographic column: HP ~ innowax, model 30m × 0.32mm, 0.50 μm;
Injector temperature 270 DEG C,
Split ratio 1:60,
Detector temperature 330 DEG C,
Column temperature is 60 DEG C and keeps 0 minute, with the ramp to 160 DEG C of 20 DEG C per minute, keeps 1 minute, then with the ramp to 180 DEG C of 2 DEG C per minute, keeps 20 minutes;
Post flow is 3.0mL/min;
Number of theoretical plate calculates should be not less than 10000 by methyl oleate peak.
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