CN112763601A - Method for measuring epoxypropanol in glycerine enema raw material - Google Patents
Method for measuring epoxypropanol in glycerine enema raw material Download PDFInfo
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- CN112763601A CN112763601A CN202011548556.6A CN202011548556A CN112763601A CN 112763601 A CN112763601 A CN 112763601A CN 202011548556 A CN202011548556 A CN 202011548556A CN 112763601 A CN112763601 A CN 112763601A
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- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 title claims abstract description 132
- 235000011187 glycerol Nutrition 0.000 title claims abstract description 54
- GJOWSEBTWQNKPC-UHFFFAOYSA-N 3-methyloxiran-2-ol Chemical compound CC1OC1O GJOWSEBTWQNKPC-UHFFFAOYSA-N 0.000 title claims abstract description 41
- 239000002994 raw material Substances 0.000 title claims abstract description 27
- 241000792859 Enema Species 0.000 title claims abstract description 24
- 239000007920 enema Substances 0.000 title claims abstract description 24
- 229940095399 enema Drugs 0.000 title claims abstract description 24
- 238000000034 method Methods 0.000 title claims abstract description 23
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 39
- 239000002904 solvent Substances 0.000 claims abstract description 8
- 238000012360 testing method Methods 0.000 claims abstract description 8
- 238000004817 gas chromatography Methods 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims description 29
- 239000013558 reference substance Substances 0.000 claims description 15
- CTKINSOISVBQLD-UHFFFAOYSA-N Glycidol Chemical compound OCC1CO1 CTKINSOISVBQLD-UHFFFAOYSA-N 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 8
- 238000005303 weighing Methods 0.000 claims description 7
- 238000007865 diluting Methods 0.000 claims description 6
- 239000002202 Polyethylene glycol Substances 0.000 claims description 5
- QUMITRDILMWWBC-UHFFFAOYSA-N nitroterephthalic acid Chemical group OC(=O)C1=CC=C(C(O)=O)C([N+]([O-])=O)=C1 QUMITRDILMWWBC-UHFFFAOYSA-N 0.000 claims description 5
- 229920001223 polyethylene glycol Polymers 0.000 claims description 5
- 239000012088 reference solution Substances 0.000 claims description 5
- 230000005526 G1 to G0 transition Effects 0.000 claims description 4
- 238000010812 external standard method Methods 0.000 claims description 3
- 239000000523 sample Substances 0.000 claims description 3
- 239000012488 sample solution Substances 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims 1
- 239000012528 membrane Substances 0.000 claims 1
- 238000001514 detection method Methods 0.000 abstract description 13
- 238000011084 recovery Methods 0.000 abstract description 9
- 238000000926 separation method Methods 0.000 abstract description 3
- 238000004458 analytical method Methods 0.000 abstract 1
- 238000003908 quality control method Methods 0.000 abstract 1
- 239000011550 stock solution Substances 0.000 description 8
- 238000002360 preparation method Methods 0.000 description 4
- 239000003814 drug Substances 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 239000012085 test solution Substances 0.000 description 3
- QCDWFXQBSFUVSP-UHFFFAOYSA-N 2-phenoxyethanol Chemical compound OCCOC1=CC=CC=C1 QCDWFXQBSFUVSP-UHFFFAOYSA-N 0.000 description 2
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 235000013305 food Nutrition 0.000 description 2
- 235000003599 food sweetener Nutrition 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- 229960005323 phenoxyethanol Drugs 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000003765 sweetening agent Substances 0.000 description 2
- 206010010774 Constipation Diseases 0.000 description 1
- FBPFZTCFMRRESA-KVTDHHQDSA-N D-Mannitol Chemical group OC[C@@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-KVTDHHQDSA-N 0.000 description 1
- 229930195725 Mannitol Natural products 0.000 description 1
- 241001465754 Metazoa Species 0.000 description 1
- 206010028980 Neoplasm Diseases 0.000 description 1
- 241000208125 Nicotiana Species 0.000 description 1
- 235000002637 Nicotiana tabacum Nutrition 0.000 description 1
- 206010040880 Skin irritation Diseases 0.000 description 1
- 239000002250 absorbent Substances 0.000 description 1
- 230000002745 absorbent Effects 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000000172 allergic effect Effects 0.000 description 1
- 208000010668 atopic eczema Diseases 0.000 description 1
- 201000011510 cancer Diseases 0.000 description 1
- 230000000711 cancerogenic effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000009982 effect on human Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000037406 food intake Effects 0.000 description 1
- 231100000024 genotoxic Toxicity 0.000 description 1
- 230000001738 genotoxic effect Effects 0.000 description 1
- 239000003230 hygroscopic agent Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 230000000968 intestinal effect Effects 0.000 description 1
- 239000008141 laxative Substances 0.000 description 1
- 230000002475 laxative effect Effects 0.000 description 1
- 229910052943 magnesium sulfate Inorganic materials 0.000 description 1
- 235000019341 magnesium sulphate Nutrition 0.000 description 1
- 239000000594 mannitol Substances 0.000 description 1
- 235000010355 mannitol Nutrition 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 210000004400 mucous membrane Anatomy 0.000 description 1
- 210000005036 nerve Anatomy 0.000 description 1
- 239000000820 nonprescription drug Substances 0.000 description 1
- 239000002674 ointment Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
- 238000011002 quantification Methods 0.000 description 1
- 210000002345 respiratory system Anatomy 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 230000036556 skin irritation Effects 0.000 description 1
- 231100000475 skin irritation Toxicity 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000000829 suppository Substances 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
Images
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
Abstract
The invention provides a method for measuring epoxypropanol in a glycerine enema raw material, which is mainly used for measuring the epoxypropanol in the glycerine enema raw material by a gas chromatography, wherein a sample adopts methanol as a solvent, so that the method is safe and has strong applicability, and the sample treatment method is convenient and rapid. The analytical method is simple, convenient and quick, has strong separation capability, accurate quantitative result and high recovery rate, the detection limit is 0.32ng, which is equivalent to 0.00008 percent of the test concentration, the quantitative limit is 0.79ng, which is equivalent to 0.00020 percent of the test concentration, the detection requirement of 0.002 percent of the epoxy propanol limit in ICH M7 is met, the quality control standard of the enema raw material is perfected, and the safety of the enema (containing glycerol) product is improved.
Description
Technical Field
The invention relates to a method for measuring epoxypropanol in a glycerine enema raw material, in particular to a method for measuring epoxypropanol in a glycerine enema raw material by using a gas chromatography.
Background
The name of glycerine enema is as follows: glycerin inema is divided into two preparations, one is a glycerol preparation, the other is a mannitol and magnesium sulfate preparation, wherein the Glycerine-containing Glycerine is most widely applied, and the Glycerine-containing Glycerine is a laxative over-the-counter medicine which is mainly used for treating children and elderly people with weak constitution and constipation. It can lubricate and irritate intestinal wall, soften stool, and make it easy to discharge.
Glycerol (Glycerin, CAS number: 56-81-5), also known as glycerol, has the molecular formula: c3H8O3Glycerol is widely used in the industries of medicine, food, paper, cosmetics, tanning, photography, printing, metal processing, electrical materials, rubber, and the like. In medicine, it is used to prepare various preparations, solvents, hygroscopic agents, antifreezing agents and sweetening agents, and is formulated into external ointment or suppository. Are used in the food industry as sweeteners, moisture absorbents for tobacco agents and solvents. Glycerol production processes can be divided into two main categories: one is a method using natural oil as raw material, and the obtained glycerol is commonly called natural glycerol; the other is a synthesis method using propylene as a raw material, and the obtained glycerol is commonly called synthetic glycerol. The epoxypropanol is used as an important intermediate for synthesizing the glycerol, is mainly generated by intramolecular dehydration of the glycerol at high temperature, and comprises the following reaction steps:
glycidol (Glycidol, CAS number 556-52-5), also known as Glycidol, has the molecular formula: c3H6O2The compound belongs to 2A substances in IARC (2000) classification of the international research center for cancer, and animal experiments prove that the compound has carcinogenic effect and may also have the same effect on human bodies. Epoxypropanol is harmful to the body by inhalation, ingestion, or transdermal absorption. The vapor or mist is irritating to the eyes, mucous membranes and upper respiratory tract. It has skin irritation. Has effect in inhibiting central nerve. Prolonged repeated exposure is allergic to certain sensitive individuals. The acceptable limit for epoxypropanol (lifetime AI) was 4 μ g/day as received in ICH M7(R1) Appendix 3(Appendix 3) version step 5. According toThe instruction principle note6 has a formula (as follows) for calculating the non-lifetime acceptable dose (less-than-life acceptable doses), which is a disposable medicine, the Total number of treatment time (Total of treatment days) is calculated according to less than 1 month (calculated according to 30 days), and the corresponding safety Factor (Sfety Factor) is 10. The estimated non-lifetime acceptable dose was 340 μ g/day.
The daily dosage of the product is that the maximum specification of the product is 20ml per bottle (containing 0.625g/ml of glycerin), the limit of the epoxy propanol in the glycerin is 340 mug/20 ml/0.625g/ml and 27.2 mug/g is 0.00272%, and the limit of the epoxy propanol in the glycerin raw material is strictly considered to be 0.002%.
Glycerol is used as a raw material of glycerine enema and the proportion in glycerine enema is as high as 55.6% (g: g), and glycidol is one of products of synthetic glycerine, and is likely to remain in glycerine, and if it contains excessive glycidol, it is likely to cause great harm to users. It is therefore important to monitor the amount of glycidol in the glycerine enema feed. Through inquiry, the fact that a detection Method (NIOSH Method 1608) for detecting the epoxypropanol in the glycerine enema raw material is relatively laggard by the national institute of occupational safety and health is found, the detection capability and the separation capability of the epoxypropanol in the glycerine enema raw material cannot meet the requirements, and therefore, the development of a Method for quickly and accurately detecting the epoxypropanol in the glycerine enema raw material is necessary.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a method for measuring epoxypropanol in a glycerine enema raw material.
The problems of high peak time of epoxypropanol in gas phase and serious interference of solvent and glycerin are successfully solved by screening conditions such as chromatographic columns, solvents, gradient programs and the like.
The invention provides a method for measuring epoxypropanol in a glycerine enema raw material, which has the specific technical scheme that:
taking about 8-12 g of glycerol raw material, precisely weighing, placing in a 25ml measuring flask, dissolving with methanol, diluting to scale, and shaking up to obtain a test solution. Precisely weighing a proper amount of epoxy propanol reference substances, adding methanol to dissolve the epoxy propanol reference substances to prepare a solution containing 6-10 mu g of epoxy propanol in each 1ml of the reference substances, and shaking up to obtain the reference substance solution.
Performing gas chromatography (in "Chinese pharmacopoeia" 2020 edition pharmacopoeia general rule 0521), using nitro terephthalic acid modified polyethylene glycol as a capillary column of stationary phase (recommended to use DB-FFAP; inner diameter 0.53mm, length 60m, film thickness 1 μm), and programming to raise temperature, wherein the initial temperature is 115-125 deg.C and maintained for 2 min; heating to 140 deg.C at a rate of 2 deg.C per minute; heating to 250 deg.C at a rate of 50 deg.C per minute, and maintaining for 10 min; then reducing the temperature to 120 ℃ at the rate of 50 ℃ per minute, and maintaining the temperature for 10 minutes; the sample inlet temperature is 190-210 ℃, the detector temperature is 240-260 ℃, the sample solution and the reference solution are precisely measured and respectively measured by 1 mu l, the measured solution and the reference solution are injected into a gas chromatograph, the chromatogram is recorded, and the content of the epoxypropanol is calculated by the peak area according to an external standard method.
The invention has the advantages that:
(1) provides a method for measuring epoxypropanol in a glycerine enema raw material, and overcomes the defects of the existing glycerine raw material detection method.
(2) The preferable capillary column (recommended to use DB-FFAP; the inner diameter is 0.53mm, the length is 60m, and the film thickness is 1 mu m) adopting the nitroterephthalic acid modified polyethylene glycol as the stationary phase has the peak emergence time of about 9.184 minutes for the epoxypropanol, about 3.104 minutes for the solvent and about 20 minutes for the glycerol, and solves the problems of faster peak emergence time and poorer separation capability for the epoxypropanol.
(3) The method for detecting the epoxypropanol in the glycerol raw material has the detection limit of 0.32ng, which is equivalent to 0.00008% of the test concentration, and the quantification limit of 0.79ng, which is equivalent to 0.00020% of the test concentration, and meets the detection requirement of 0.002% of the limit of the epoxypropanol in the glycerol.
(4) The method is adopted to detect the epoxypropanol, the concentration of the epoxypropanol is in a good linear relation within the range of 0.791 mu g/ml-15.821 mu g/ml, and the linear equation is as follows: y 0.4387x +0.1097 with a correlation coefficient of 1.000. The average recovery of the 9 groups of samples was 98.9%.
Therefore, the method provided by the invention is a method for determining epoxypropanol in the glycerine enema raw material, provides an accurate, reliable and simple method for determining epoxypropanol therein, and can meet the detection requirement of the epoxypropanol which is a genotoxic impurity in the glycerine enema raw material.
Drawings
Fig. 1 is a blank solvent, fig. 2 is a control solution, fig. 3 is a sample with 100% concentration recovery rate, fig. 4 is a limit spectrum, and fig. 5 is a limit spectrum.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention are clearly and completely described, and it is obvious that the described embodiments are a part of the embodiments of the present invention, but not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1: recovery rate experiment for detecting phenoxyethanol in glycerol raw material
The instrument comprises the following steps: agilent 7890B gas chromatograph
Chromatographic conditions are as follows:
a capillary column (recommended to use DB-FFAP; 0.53mm multiplied by 60m,1 mu m) with fixed phase (or fixed phase with similar polarity) modified by polyethylene glycol modified by nitro terephthalic acid, and raising the temperature by program, wherein the initial temperature is 120 ℃ and is maintained for 2 minutes; heating to 140 deg.C at a rate of 2 deg.C per minute; heating to 250 deg.C at a rate of 50 deg.C per minute, and maintaining for 10 min; then reducing the temperature to 120 ℃ at the rate of 50 ℃ per minute, and maintaining the temperature for 10 minutes; the injection port temperature is 200 ℃, and the detector temperature is 250 ℃.
The experimental steps are as follows:
reference stock solution: taking 20mg of epoxy propanol reference substance, precisely weighing, placing in a 25ml measuring flask, dissolving with methanol and diluting to scale, shaking up, precisely weighing 5ml of the above solution, placing in a 100ml volumetric flask, dissolving with methanol and diluting to scale, shaking up, and using as reference substance stock solution.
Control solution: precisely measuring 5ml of the reference stock solution, placing the reference stock solution in a 25ml measuring flask, dissolving the reference stock solution with methanol, diluting the reference stock solution to a scale, and shaking the reference stock solution uniformly to obtain a reference solution.
Test solution: about 10g of the product is precisely weighed, placed in a 25ml measuring flask, dissolved and diluted to the scale with methanol, and shaken up to be used as a test solution.
Recovery rate solution: about 10g of glycerol is taken and placed in a 25ml measuring flask to prepare 9 parts in parallel, 2.5ml, 5ml and 7.5ml of reference substance stock solutions are respectively added, dissolved and diluted to the scale by methanol and shaken up to be used as 50 percent, 100 percent and 150 percent test substance solutions, and 3 parts are prepared at each concentration.
And (3) taking 1 mu l of each solution, injecting the solution into a gas chromatograph, recording a chromatogram, and calculating the recovery rate by peak area according to an external standard method.
Results of recovery test
As a result: the average value of the recovery rates of the 9 groups is 98.9%, the RSD value is 1.16%, the maximum value is 100.48%, the minimum value is 97.04%, and the recovery rates meet the requirement.
Example 2: detection limit and quantitative limit experiment for detecting phenoxyethanol in glycerol raw material
The instrument comprises the following steps: agilent 7890B gas chromatograph
Chromatographic conditions are as follows:
a capillary column (DB-FFAP is recommended; the inner diameter is 0.53mm, the length is 60m, and the film thickness is 1 mu m) taking nitroterephthalic acid modified polyethylene glycol as a stationary phase, and raising the temperature by a program, wherein the initial temperature is 120 ℃ and is maintained for 2 minutes; heating to 140 deg.C at a rate of 2 deg.C per minute; heating to 250 deg.C at a rate of 50 deg.C per minute, and maintaining for 10 min; then reducing the temperature to 120 ℃ at the rate of 50 ℃ per minute, and maintaining the temperature for 10 minutes; the injection port temperature is 200 ℃, and the detector temperature is 250 ℃.
The experimental steps are as follows:
control solution: precisely weighing 20mg of epoxypropanol reference substance, placing in 25ml volumetric flask, adding methanol to dissolve and dilute to scale, shaking, precisely transferring 1ml of the above solution, placing in 100ml volumetric flask, adding methanol to dilute to scale, shaking to obtain reference substance solution
And taking the reference substance solution, diluting the reference substance solution step by step until the peak signal-to-noise ratio of the epoxypropanol is about 10, and taking the reference substance solution as a quantitative limiting solution, and taking the reference substance solution as a detection limiting solution when the peak signal-to-noise ratio of the epoxypropanol is about 3. And respectively taking 1 mu l of the quantitative limit solution and the detection limit solution, injecting the solutions into a gas chromatograph, recording a chromatogram, and respectively inspecting the detection limit and the quantitative limit.
Test results of detection limit and quantitative limit
The above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments can still be modified, or some technical features of the foregoing embodiments can be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (4)
1. A method for measuring epoxypropanol in a glycerine enema raw material is characterized by comprising the following steps: using gas chromatography, wherein the stationary phase of the capillary column is polyethylene glycol modified with nitro terephthalic acid, the inner diameter of the column is 0.53mm, the length is 60m, and the thickness of the liquid membrane is 1 μm;
the solvent is methanol;
the temperature raising procedure is that the initial temperature is 115 ℃ to 125 ℃, and the temperature is kept for 2 minutes; heating to 140 deg.C at a rate of 2 deg.C per minute; heating to 250 deg.C at a rate of 50 deg.C per minute, and maintaining for 10 min; then reducing the temperature to 120 ℃ at the rate of 50 ℃ per minute, and keeping the temperature for 10 minutes;
the sample inlet temperature is 190-210 ℃, the detector temperature is 240-260 ℃, the sample solution and the reference solution are precisely measured and respectively measured by 1 mu l, the measured solution and the reference solution are injected into a gas chromatograph, the chromatogram is recorded, and the content of the epoxypropanol is calculated by the peak area according to an external standard method.
2. The method for determining glycidol in a glycerine enema raw material as claimed in claim 1, wherein the test samples are: taking 8-12 g of glycerol raw material, precisely weighing, placing in a 25ml measuring flask, dissolving with methanol and diluting to scale.
3. The method for determining glycidol in a glycerine enema feed as claimed in claim 1, wherein said control samples are: and precisely weighing a proper amount of epoxy propanol reference substances, and adding methanol to dissolve the epoxy propanol reference substances to prepare a solution containing 6-10 mu g of epoxy propanol in each 1 ml.
4. The method for determining glycidol in a glycerine enema feed as claimed in claim 1, wherein said capillary column is DB-FFAP.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103242266A (en) * | 2013-05-15 | 2013-08-14 | 邵阳学院 | Method for synthetizing glycidol |
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| CN105548414A (en) * | 2015-12-24 | 2016-05-04 | 杭州嘉伟生物制品有限公司 | BDDE residual quantity detection method |
| CN109975467A (en) * | 2017-12-28 | 2019-07-05 | 贵州中烟工业有限责任公司 | The measuring method of epoxy prapanol in a kind of cigarette mainstream flue gas |
| US20210017142A1 (en) * | 2018-03-28 | 2021-01-21 | Green Lizard Technologies Ltd | Process for the preparation of glycidol |
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2020
- 2020-12-24 CN CN202011548556.6A patent/CN112763601A/en active Pending
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|---|---|---|---|---|
| CN103242266A (en) * | 2013-05-15 | 2013-08-14 | 邵阳学院 | Method for synthetizing glycidol |
| CN104807911A (en) * | 2015-05-13 | 2015-07-29 | 浙江中一检测研究院股份有限公司 | Method for testing glycidol in air and waste gas |
| CN105548414A (en) * | 2015-12-24 | 2016-05-04 | 杭州嘉伟生物制品有限公司 | BDDE residual quantity detection method |
| CN109975467A (en) * | 2017-12-28 | 2019-07-05 | 贵州中烟工业有限责任公司 | The measuring method of epoxy prapanol in a kind of cigarette mainstream flue gas |
| US20210017142A1 (en) * | 2018-03-28 | 2021-01-21 | Green Lizard Technologies Ltd | Process for the preparation of glycidol |
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