CN107607632A - The method of residual solvent in extraction of ginkgo biloba leaves by headspace gas - Google Patents
The method of residual solvent in extraction of ginkgo biloba leaves by headspace gas Download PDFInfo
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- CN107607632A CN107607632A CN201710667192.5A CN201710667192A CN107607632A CN 107607632 A CN107607632 A CN 107607632A CN 201710667192 A CN201710667192 A CN 201710667192A CN 107607632 A CN107607632 A CN 107607632A
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Abstract
The present invention relates to a kind of method of residual solvent in extraction of ginkgo biloba leaves by headspace gas bulk drug, comprise the following steps：(1) chromatographic condition and system suitability；(2) preparation of reference substance solution and need testing solution；(3) determine：Reference substance, test sample difference headspace sampling injection gas chromatograph, external standard method calculate the content of hexamethylene, ethanol and ethyl acetate.The present invention is bright through methodology proof list, and separating degree is good, and test limit, quantitative limit, linear, stability, average recovery etc. meet the requirements, and can be used for the residues detection of ginkgo biloba p.e cyclohexane, ethanol and ethyl acetate.The invention provides a kind of analysis method that can easy, fast and accurately detect ginkgo biloba p.e dissolvent residual, used suitable for industrialized production, there is larger application value.
Description
Technical field
The present invention relates to Chinese medicine, and in particular to the detection method of Chinese medical extract residual solvent, more particularly to a kind of head space
The method of residual solvent in gas chromatography measure ginkgo biloba p.e.
Background technology
With more and more stricter to quality requirements such as food, medicines, the product in production process using organic solvent is entered
The requirement more and more higher of row residual solvent analysis detection.Ginkgo biloba p.e is extracted by ginkgo leaf and obtained, for treating blood stasis type
Dizziness caused by the obstruction of qi in the chest (coronary disease and angina pectoris) and the slight cerebral arteriovenous malformation of blood stasis type.It is main residual in ginkgo biloba p.e product
It is hexamethylene, ethanol and ethyl acetate to stay solvent, is not had also to the detection method of ginkgo biloba p.e organic solvent residual at present
Report.In instrument analytical method, headspace sampling system (the also known as headspace gas chromatography equipped with capillary gas chromatography technology
Method), the detection for volatile organic matter has many strong points such as sample pre-treatments are simple, sensitivity is high.It is especially this
Analysis method will only volatilize and the component of half volatilization introduces pillar, can also avoid the dirt of nonvolatile confrontation system in sample
Dye, therefore, headspace gas chromatography method are considered as one of better method for analyzing volatile organic matter.But this method energy
The no detection for ginkgo biloba p.e organic solvent residual needs further research and design, and this is for ensuring ginkgo biloba p.e
Quality have important value.
The content of the invention
The technical problems to be solved by the invention are to overcome above-mentioned weak point, and research and design one kind can be easy, fast
The method of speed, accurately detection ginkgo biloba p.e bulk drug dissolvent residual.
The invention provides a kind of method of residual solvent in extraction of ginkgo biloba leaves by headspace gas.
The technical solution adopted by the present invention：Ginkgo biloba p.e is taken to be added in right amount in headspace gas chromatography 20ml ml headspace bottles,
5mlDMSO (dimethyl sulfoxide (DMSO)) ultrasonic dissolution is pipetted with pipette, is made into the solution that concentration is 40mg/ml, it is molten as test sample
Liquid；In addition, precision weighs chromatographic grade hexamethylene, ethanol, ethyl acetate in right amount into volumetric flask respectively, add DMSO that every 1mL is made
The respectively mixed solution containing 0.15mg, 0.2mg, 0.2mg, pipette, which pipettes, is used as reference substance in solution 5ml to 20ml ml headspace bottles
Solution, gas chromatograph detection, test sample hexamethylene, ethanol, ethyl acetate content are calculated with quantified by external standard method, final to calculate
Go out each Determination of Residual Organic Solvents in ginkgo biloba p.e bulk drug.
Specifically, the inventive method comprises the following steps：
(1) chromatographic condition and system suitability：Chromatographic column is 6%- cyanogen propyl group phenyl -94%- dimethyl siloxanes
Copolymer capillary column, carrier gas are high pure nitrogen, and detector is hydrogen ion flame (FID) detector, reference substance solution and confession examination
Product solution headspace sampling, 200-220 DEG C of injector temperature, 200-280 DEG C of detector temperature, 30-230 DEG C of column temperature, temperature programming,
Hexamethylene, ethanol, ethyl acetate peak separating degree are more than 1.5, and each peak symmetry is good；
(2) preparation of reference substance solution and need testing solution：(a) reference substance solution：Precision weighs chromatographic grade hexamethylene respectively
Alkane, ethanol, appropriate ethyl acetate, add DMSO that mixed solutions of every 1mL respectively containing about 0.15mg, 0.2mg, 0.2mg, pipette is made
Pipette the 5ml mixed solutions and reference substance solution is used as into 20ml ml headspace bottles；
(b) need testing solution：Accurately weighed ginkgo biloba p.e into 20ml ml headspace bottles, is taken with pipette in right amount
5mlDMSO ultrasounds make dissolving, and it is 40mg/ml to make ginkgo biloba p.e concentration, is shaken up, as need testing solution；
(3) determine：Reference substance and test sample difference headspace sampling 1ml, inject gas chromatograph, measure, external standard method calculates
The content of hexamethylene, ethanol and ethyl acetate, finally calculate each Determination of Residual Organic Solvents in ginkgo biloba p.e.
The similar stationary phase of step described in the inventive method (1) chromatographic column is DB-624, column length 30m, column internal diameter 0.53mm, thin
3 μm of film thickness.
200-220 DEG C of the injector temperature, 200-280 DEG C of detector temperature, 30-230 DEG C of column temperature.
The method of described program heating：40 DEG C of holding 10min, then 230 DEG C are risen to 20 DEG C/min heating rate, keep
5min。
The present inventor have passed through research, design and improves and tests for the various essential conditions of this detection method, breach
The routine of this area：
(1) selection of solvent：Headspace gas chromatography common solvent is water and DMF (DMF), but water
The service life of chromatographic column can be shortened.And according to the principle of " similar to mix ", only in uniform system, it could obtain preferably
Analytical precision and accuracy, and ginkgo biloba p.e is not soluble in water.In addition, DMF at high temperature facile hydrolysis formic acid with
Dimethyl amine, it is possible to which meeting Interference Detection, the present invention abandon DMF, by the research selection DMSO that stability in use is good, boiling point is high
Good result is obtained as solvent.In use, DMSO can not only sample dissolution, and with hexamethylene, ethanol, ethyl acetate
It can dissolve each other, make sample treatment simple and convenient.
(2) selection of chromatographic column：Residual solvent in ginkgo biloba p.e has multiple kinds, each not phase of their boiling point
Together, such as 80.7 DEG C of hexamethylene boiling point, 78 DEG C of ethanol, 77 DEG C of ethyl acetate.The boiling point of particularly ethanol and ethyl acetate extremely connects
Closely.It may require that column temperature condition is harsher if selection uses nonpolar capillary column, not only extend analysis time, and point
It is relatively low from spending, influence accuracy of measurement.6%- cyanogen propyl group phenyl -94%- two of the present invention through research selection using middle polarity
Methylpolysiloxane Copolymer capillary column, to improve specificity, it is DB-624 to determine similar stationary phase, the results showed that, three kinds are residual
Stay solvent separating degree preferably, analysis time it is shorter, reached easy, fast and accurately effect.
The advantages of headspace injection method is only to take ml headspace bottle internal upper part gas to be injected into gas chromatograph to carry out separation determination,
Disturbing factor is less, and measurement result is accurate.
The present invention is detected with headspace gas chromatography to ginkgo biloba p.e bulk drug, is accurately detected ginkgo
Each Determination of Residual Organic Solvents in leaf extract.(see embodiment 1-3)
Detection method is bright through methodology proof list, the separation of hexamethylene, ethanol, ethyl acetate and solvent peak DMSO
Work well.In terms of the investigation that the methods of test limit, quantitative limit, linear, stability, average recovery is learned, meet quantitative
The requirement of measure.The invention provides a kind of analysis that can easy, fast and accurately detect ginkgo biloba p.e dissolvent residual
Method.Used suitable for industrialized production, there is larger application value.
Embodiment
With reference to embodiment, the present invention is further detailed explanation.Embodiment provides by way of example, not
It is construed as limiting the invention.
Following examples are raw materials used and reagent is by being commercially available.
The sample detection of embodiment 1 and detection method repeated experiment
The preparation of ginkgo biloba p.e：
Ginkgo leaf 100kg is taken, adds hydrous ethanol refluxing extraction 2 times, 80% alcohol reflux for adding 750L for the first time carries
2h is taken, adds 650L 70% alcohol reflux extraction 2h for the second time, third time adds 500L water refluxing extraction 2h, 2 times by before
Ethanol extract merges, and is concentrated under reduced pressure into no alcohol taste, adds 200L cold water, stir, stand overnight, and filters, and collects filter
Liquid, merge with aqueous extract, by kymene 5L D-101 resins, wash 100L, collect, it is stand-by, then with 70% ethanol elution
70L, is concentrated under reduced pressure into 10L, and ethyl acetate extracts 3 times, and each extraction quantity is respectively 12L, 10L, 8L, collect respectively extract and
Raffinate, extract are concentrated under reduced pressure into no ethyl acetate taste, place stand-by；By raffinate and above-mentioned water lotion conjunction after crossing polyamide
And by 20L polyamides, wash 40L.Again with 70% ethanol elution 40L, closed with above-mentioned ethyl acetate extraction concentrate
And no alcohol taste is concentrated under reduced pressure into, extracted 2 times with hexamethylene, add hexamethylene 600ml every time, collected aqueous phase, be concentrated under reduced pressure into
It is dry, produce.(1) preparation of need testing solution：Take in ginkgo biloba p.e 0.2g to 20ml ml headspace bottles, it is accurately weighed, it is parallel to take 6
Part sample, pipette, which pipettes 5mlDMSO ultrasounds, makes dissolving, and it is 40mg/ml to make ginkgo biloba p.e concentration, is shaken up, as trying
Product solution；
(2) preparation of reference substance solution：Precision weighs chromatographic grade hexamethylene, ethanol, appropriate ethyl acetate respectively, adds DMSO
Mixed solutions of every 1mL respectively containing about 0.15mg, 0.2mg, 0.2mg is made, by the use of pipette pipette in 5ml to 20ml ml headspace bottles as
Reference substance solution；
(3) determine：
Instrument：Shimadzu GC-2010 gas chromatographs, Shimadzu GCsolution work stations, the full Pu QPT-300G type nitrogen in Shanghai
Hydrogen sky all-in-one, Mei Teletuo benefit AL204 electronic balances.
Chromatographic condition：Chromatographic column is DB-624 capillary columns, column length 30m, column internal diameter 0.53mm, 3 μm of film thickness；Carrier gas
For high pure nitrogen；Detector is hydrogen ion flame (FID) detector；210 DEG C of injector temperature, 35-230 DEG C of column temperature, program liter
Temperature, 35 DEG C of holding 10min, rises to 230 DEG C with 20 DEG C/min heating rate, keeps 3min；250 DEG C of detector temperature.
Assay method：Reference substance solution, need testing solution difference headspace sampling 1ml, injects gas chromatograph, determines, outside
Mark method calculates the content of hexamethylene, ethanol and ethyl acetate, finally calculates each Determination of Residual Organic Solvents in ginkgo biloba p.e.
The testing result and method repeatability result of the test sample hexamethylene of table 1, ethanol and Determination of Residual Ethyl Acetate (%)
| Sequence number | Hexamethylene | Ethanol | Ethyl acetate |
| 1 | 0.0521 | 0.0992 | 0.0356 |
| 2 | 0.0521 | 0.0991 | 0.0363 |
| 3 | 0.0522 | 0.0992 | 0.0358 |
| 4 | 0.0521 | 0.0989 | 0.0357 |
| 5 | 0.0520 | 0.0992 | 0.0359 |
| 6 | 0.0521 | 0.0990 | 0.0361 |
| Average value | 0.0521 | 0.0991 | 0.0359 |
| RSD | 0.12% | 0.13% | 0.73% |
As a result show：In 6 parallel samples of ginkgo biloba p.e, hexamethylene, ethanol and Determination of Residual Ethyl Acetate average
Respectively 0.521%, 0.0991%, 0.73%.RSD is respectively 0.12%, 0.13%, 0.73%, respectively less than 2%, shows this
Method is reproducible, and the degree of accuracy is high, the detection available for ginkgo biloba p.e dissolvent residual.
The ginkgo biloba p.e sample detection of embodiment 2
The preparation of ginkgo biloba p.e：
Ginkgo leaf 100kg is taken, adds hydrous ethanol refluxing extraction 2 times, 80% alcohol reflux for adding 800L for the first time carries
2h is taken, adds 600L 70% alcohol reflux extraction 2h for the second time, third time adds 600L water refluxing extraction 2h, 2 times by before
Ethanol extract merges, and is concentrated under reduced pressure into no alcohol taste, adds 150L cold water, stir, stand overnight, and filters, and collects filter
Liquid, merge with aqueous extract, by kymene 5L D-101 resins, wash 100L, collect, it is stand-by, then with 70% ethanol elution
70L, is concentrated under reduced pressure into 10L, and ethyl acetate extracts 3 times, and each extraction quantity is respectively 12L, 10L, 8L, collect respectively extract and
Raffinate, extract are concentrated under reduced pressure into no ethyl acetate taste, place stand-by；By raffinate and above-mentioned water lotion conjunction after crossing polyamide
And by 20L polyamides, wash 40L.Again with 70% ethanol elution 40L, closed with above-mentioned ethyl acetate extraction concentrate
And no alcohol taste is concentrated under reduced pressure into, extracted 2 times with hexamethylene, add hexamethylene 800ml every time, collected aqueous phase, be concentrated under reduced pressure into
It is dry, produce.
Reference substance solution is the same as embodiment 1；
Need testing solution：Take in ginkgo biloba p.e 0.2g to 20ml ml headspace bottles, it is accurately weighed, it is parallel to take 3 parts of samples, move
Liquid pipe, which pipettes 5mlDMSO ultrasounds, makes dissolving, and it is 40mg/ml to make ginkgo biloba p.e concentration, is shaken up, as need testing solution；
Chromatographic condition is the same as embodiment 1；
Assay method：Reference substance solution, need testing solution difference headspace sampling 1ml, injects gas chromatograph, determines, outside
Mark method calculates the content of hexamethylene, ethanol and ethyl acetate, finally calculates each Determination of Residual Organic Solvents in ginkgo biloba p.e.
The testing result of the test sample hexamethylene of table 2, ethanol and Determination of Residual Ethyl Acetate (%)
| Sequence number | Hexamethylene | Ethanol | Ethyl acetate |
| 1 | 0.0543 | 0.105 | 0.0372 |
| 2 | 0.0545 | 0.104 | 0.0371 |
| 3 | 0.0551 | 0.106 | 0.0372 |
| Average value | 0.0546 | 0.105 | 0.0372 |
| RSD | 0.76% | 0.95% | 0.16% |
Conclusion：To the ginkgo biloba p.e prepared again, detect three parallel samples, hexamethylene, ethanol, ethyl acetate
Residual quantity average is respectively 0.0546%, 0.105%, 0.0372%.RSD is respectively less than 2%, again shows that this method can be accurate
Determine dissolvent residual.
The ginkgo biloba p.e sample detection of embodiment 3
The preparation of ginkgo biloba p.e：
Ginkgo leaf 100kg is taken, adds hydrous ethanol refluxing extraction 2 times, 80% alcohol reflux for adding 600L for the first time carries
2h is taken, adds 700L 70% alcohol reflux extraction 2h for the second time, third time adds 550L water refluxing extraction 2h, 2 times by before
Ethanol extract merges, and is concentrated under reduced pressure into no alcohol taste, adds 180L cold water, stir, stand overnight, and filters, and collects filter
Liquid, merge with aqueous extract, by kymene 5L D-101 resins, wash 100L, collect, it is stand-by, then with 70% ethanol elution
70L, is concentrated under reduced pressure into 10L, and ethyl acetate extracts 3 times, and each extraction quantity is respectively 12L, 10L, 8L, collect respectively extract and
Raffinate, extract are concentrated under reduced pressure into no ethyl acetate taste, place stand-by；By raffinate and above-mentioned water lotion conjunction after crossing polyamide
And by 20L polyamides, wash 40L.Again with 70% ethanol elution 40L, closed with above-mentioned ethyl acetate extraction concentrate
And no alcohol taste is concentrated under reduced pressure into, extracted 2 times with hexamethylene, add hexamethylene 620ml every time, collected aqueous phase, be concentrated under reduced pressure into
It is dry, produce.
Reference substance solution is the same as embodiment 1；
Need testing solution：Take in ginkgo biloba p.e 0.2g to 20ml ml headspace bottles, it is accurately weighed, it is parallel to take 3 parts of samples, move
Liquid pipe, which pipettes 5mlDMSO ultrasounds, makes dissolving, and it is 40mg/ml to make ginkgo biloba p.e concentration, is shaken up, as need testing solution；
Chromatographic condition is the same as embodiment 1；
Assay method：Reference substance solution, need testing solution difference headspace sampling 1ml, injects gas chromatograph, determines, outside
Mark method calculates the content of hexamethylene, ethanol and ethyl acetate, finally calculates each Determination of Residual Organic Solvents in ginkgo biloba p.e.
The testing result of the test sample hexamethylene of table 3, ethanol and Determination of Residual Ethyl Acetate (%)
Conclusion：The ginkgo biloba p.e prepared to third time, detect three parallel samples, hexamethylene, ethanol, ethyl acetate
Residual quantity average be respectively 0.0494%, 0.105%, 0.0352%.RSD is respectively less than 2%, continuously sample preparation three times and
Detection can confirm that this method can be with Accurate Determining dissolvent residual.
The ginkolide B dissolvent residual detecting system employment and suitability test (E ＆ ST) of the present invention of embodiment 4
Instrument：Shimadzu GC-2010 gas chromatographs, Shimadzu GCsolution work stations, the full Pu QPT-300G type nitrogen in Shanghai
Hydrogen sky all-in-one, Mei Teletuo benefit AL204 electronic balances.
The preparation of reference substance solution：Precision weighs chromatographic grade hexamethylene, ethanol, appropriate ethyl acetate respectively, adds DMSO systems
Mixed solution into every 1mL respectively containing about 0.15mg, 0.2mg, 0.2mg, as reference substance solution；
Chromatographic condition：Chromatographic column is 6%- cyanogen propyl group phenyl -94%- dimethylsiloxane copolymer capillary columns, column length
30m, column internal diameter 0.53mm, 3 μm of film thickness；Carrier gas is high pure nitrogen；Detector is hydrogen ion flame (FID) detector；Enter
220 DEG C of sample mouth temperature, 35-230 DEG C of column temperature, temperature programming, 35 DEG C of holding 10min, 230 are risen to 20 DEG C/min heating rate
DEG C, keep 3min；250 DEG C of detector temperature.
Assay method：Precision measures the μ L of reference substance solution 0.5, direct injected injection gas chromatograph, records chromatogram, color
Peak sequence is followed successively by that hexamethylene, ethyl acetate, ethanol, DMSO peak shapes are symmetrical, and separating degree is good in spectrogram, reach 1.5 with
On.
The detection method test limit of embodiment 5 is tested
Reference substance solution is prepared, the concentration for making hexamethylene, ethanol and ethyl acetate is respectively 0.001mg/ml, 0.002mg/
Ml, 0.001mg/ml, take 0.5 μ L sample detections, and each peak signal to noise ratio is more than 3.
The test limit result of table 4
| Reference substance composition | Concentration (mg/ml) | Signal to noise ratio | Detection limit (μ g) |
| Methanol | 0.001 | ＞ 3 | 0.0005 |
| Ethanol | 0.002 | ＞ 3 | 0.001 |
| Ethyl acetate | 0.001 | ＞ 3 | 0.0005 |
Signal to noise ratio result shows, when sample size is 0.5 μ L, the content of methanol, ethanol and ethyl acetate is not low in test sample
In 0.0005 μ g, 0.001 μ g, 0.0005 μ g can be detected, similarly, when ginkolide B sampling amount is 200mg, methanol, ethanol
It is more than 0.0025%, 0.005% with the residual quantity of ethyl acetate, 0.0025% can be detected.
The detection method quantitative limit of embodiment 6 is tested
Contrast solution is prepared, the concentration for making methanol, ethanol and ethyl acetate is respectively 0.005mg/ml, 0.01mg/ml,
0.005mg/ml, takes 0.5 μ L sample detections, and each peak signal to noise ratio is more than 10.
The quantitative limit result of table 5
| Reference substance composition | Concentration (mg/ml) | Signal to noise ratio | Detection limit (μ g) |
| Methanol | 0.005 | ＞ 10 | 0.0025 |
| Ethanol | 0.01 | ＞ 10 | 0.005 |
| Ethyl acetate | 0.005 | ＞ 10 | 0.0025 |
Signal to noise ratio result shows, when sample size is 0.5 μ L, the content of methanol, ethanol and ethyl acetate is not low in test sample
It can be adapted to quantitative calculating in 0.0025 μ g, 0.005 μ g, 0.0025 μ g, similarly, when ginkolide B sampling amount is 200mg, first
The residual quantity of alcohol, ethanol and ethyl acetate is more than 0.0125%, 0.025%, and 0.0125% is adapted to quantitative calculate.
The Linear Experiment of the detection method of embodiment 7
Prepare mixing reference substance mother liquor (often the μ g containing methanol 1006, the μ g of ethanol 1268, the μ g of ethyl acetate 1028 in l ml).
From mixing reference substance mother liquor precision pipette 5,2, l, 0.5,0.2ml, put respectively in 10ml measuring bottles, while essence takes reference substance mother liquor
0.2ml puts 100ml measuring bottles, with dilution in acetonitrile and is settled to scale, as each standard curve sample, chromatographic condition with embodiment 1,
0.5 μ l direct injecteds are taken respectively, are recorded chromatogram, are measured peak area, using peak area as ordinate (y), concentration C (μ g/ml) is
Abscissa (x) carries out linear regression.It the results are shown in Table l, it is seen that each component linear relationship in its concentration range is good.
The standard curve linear regression table of table 6
| Composition | Linear equation | R values | Concentration range (μ g/ml) |
| Methanol | Y=3987.9x-14003 | 0.9999 | 2.0~503.0 |
| Ethanol | Y=5220.1x-7457.7 | 0.9999 | 2.5~634.0 |
| Ethyl acetate | Y=4321.8x-1743.7 | 0.9999 | 2.1~514.0 |
The detection method rate of recovery of embodiment 8 is tested
Absorption method is loaded using blank, methanol, ethanol and ethyl acetate, acetonitrile are separately added into by basic, normal, high three concentration
Dissolved dilution is to 10ml, and as test sample, every kind of concentration 3 is parallel, and contrast solution and detection method are the same as embodiment 1.
The average recovery experimental result of table 7
Pass through blank average recovery experimental data：This method rate of recovery is good, methanol, ethanol, ethyl acetate it is flat
The equal rate of recovery is respectively 99.6%, 99.9%, and 99.6%, RSD values are respectively 0.61%, 0.43%, 0.21%.
The instrument precision of embodiment 9 is tested
The reference substance solution of Example 1, chromatographic condition and detection method are the same as embodiment 1, continuous 6 sample detections, first
Alcohol, ethanol, the RSD of ethyl acetate peak area are respectively 0.74%, 0.17%, 0.48%, respectively less than 2%, show instrument precision
Degree is good, is adapted to this method detection.
The instrument precision result of the test of table 8
The stability experiment of the detection method of embodiment 10
Reference substance solution in Example 1 takes 0.5 μ L to detect respectively at the 0th, 2,4,6,8,24h, chromatographic condition and inspection
Survey method determines peak area with embodiment 1, and methanol, ethanol, the RSD% of ethyl acetate peak area are respectively 0.72%, 1.4%,
0.53%, show that sample is placed 24h and had good stability, can meet to detect needs.
The Detection of Stability peak area result of table 9
Claims (3)
1. a kind of method of residual solvent in extraction of ginkgo biloba leaves by headspace gas, it is characterised in that this method bag
Include the following steps：
(1) chromatographic condition and system suitability：Chromatographic column is 6%- cyanogen propyl group phenyl -94%- Dimethicone Copolyols
Thing capillary column, carrier gas are high pure nitrogen, and detector is hydrogen ion flame detector, reference substance solution and need testing solution head space
Sample introduction, temperature programming, hexamethylene, ethanol, ethyl acetate peak separating degree are more than 1.5, and each peak symmetry is good；
(2) preparation of reference substance solution and need testing solution：
(a) reference substance solution：Precision weighs chromatographic grade hexamethylene, ethanol, appropriate ethyl acetate respectively, adds DMSO that every 1mL is made
Mixed solution respectively containing about 0.15mg, 0.2mg, 0.2mg, pipette pipette the conduct into 20ml ml headspace bottles of the 5ml mixed solutions
Reference substance solution；
(b) need testing solution：Accurately weighed ginkgo biloba p.e into 20ml ml headspace bottles, takes 5mlDMSO to surpass with pipette in right amount
Sound makes dissolving, and it is 40mg/ml to make ginkgo biloba p.e concentration, is shaken up, as need testing solution；
(3) determine：Reference substance and test sample difference headspace sampling 1ml, inject gas chromatograph, measure, external standard method calculates hexamethylene
The content of alkane, ethanol and ethyl acetate, finally calculate each Determination of Residual Organic Solvents in ginkgo biloba p.e.
2. according to claim 1 in a kind of extraction of ginkgo biloba leaves by headspace gas residual solvent method, its
It is characterised by, the similar stationary phase of step (1) chromatographic column is DB-624, column length 30m, column internal diameter 0.53mm, the μ of film thickness 3
m。
3. according to claim 1 in a kind of extraction of ginkgo biloba leaves by headspace gas residual solvent method, its
It is characterised by, 200-220 DEG C of step (1) injector temperature, 200-280 DEG C of detector temperature, 30-230 DEG C of column temperature；Program
The method of heating：40 DEG C of holding 10min, then 230 DEG C are risen to 20 DEG C/min heating rate, keep 5min.
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| CN108572226A (en) * | 2018-06-04 | 2018-09-25 | 新疆维吾尔自治区分析测试研究院 | Method based on Headspace Gas Chromatography alcoholic strength low Determination of Ethanol in Drink |
| CN110627806A (en) * | 2019-09-29 | 2019-12-31 | 上海信谊百路达药业有限公司 | Bilobalide B compound and preparation method thereof |
| CN110627807A (en) * | 2019-09-29 | 2019-12-31 | 上海信谊百路达药业有限公司 | Bilobalide B raw material and preparation method thereof |
| CN111751459A (en) * | 2020-05-27 | 2020-10-09 | 济川药业集团有限公司 | Method for simultaneously detecting multiple residual solvents in sitafloxacin |
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| CN111751459A (en) * | 2020-05-27 | 2020-10-09 | 济川药业集团有限公司 | Method for simultaneously detecting multiple residual solvents in sitafloxacin |
| CN113624855A (en) * | 2020-12-29 | 2021-11-09 | 晨光生物科技集团股份有限公司 | Method for detecting residual quantity of n-hexane and acetone solvents in crystal lycopene |
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