CN114428140A - Preparation method of tert-butyl hydroquinone standard solution - Google Patents
Preparation method of tert-butyl hydroquinone standard solution Download PDFInfo
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- CN114428140A CN114428140A CN202210093127.7A CN202210093127A CN114428140A CN 114428140 A CN114428140 A CN 114428140A CN 202210093127 A CN202210093127 A CN 202210093127A CN 114428140 A CN114428140 A CN 114428140A
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- tert
- standard solution
- butyl hydroquinone
- butylhydroquinone
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- BGNXCDMCOKJUMV-UHFFFAOYSA-N Tert-Butylhydroquinone Chemical compound CC(C)(C)C1=CC(O)=CC=C1O BGNXCDMCOKJUMV-UHFFFAOYSA-N 0.000 title claims abstract description 74
- 239000004250 tert-Butylhydroquinone Substances 0.000 title claims abstract description 73
- 235000019281 tert-butylhydroquinone Nutrition 0.000 title claims abstract description 72
- 239000012086 standard solution Substances 0.000 title claims abstract description 60
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 239000002904 solvent Substances 0.000 claims abstract description 24
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000003708 ampul Substances 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 14
- DGVVWUTYPXICAM-UHFFFAOYSA-N β‐Mercaptoethanol Chemical compound OCCS DGVVWUTYPXICAM-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000001514 detection method Methods 0.000 claims abstract description 12
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 11
- 238000005303 weighing Methods 0.000 claims abstract description 11
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000001301 oxygen Substances 0.000 claims abstract description 10
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 10
- 238000007789 sealing Methods 0.000 claims abstract description 10
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims abstract description 5
- 229910052708 sodium Inorganic materials 0.000 claims abstract description 5
- 239000011734 sodium Substances 0.000 claims abstract description 5
- 239000011521 glass Substances 0.000 claims abstract description 4
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 45
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 21
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 21
- 238000005259 measurement Methods 0.000 claims description 8
- 239000000126 substance Substances 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 4
- 238000004364 calculation method Methods 0.000 claims description 2
- 230000003647 oxidation Effects 0.000 abstract description 2
- 238000007254 oxidation reaction Methods 0.000 abstract description 2
- 238000012795 verification Methods 0.000 abstract 1
- 235000013305 food Nutrition 0.000 description 8
- 238000012360 testing method Methods 0.000 description 7
- 239000003963 antioxidant agent Substances 0.000 description 6
- 239000002994 raw material Substances 0.000 description 6
- 239000000243 solution Substances 0.000 description 4
- 238000013112 stability test Methods 0.000 description 4
- 230000003078 antioxidant effect Effects 0.000 description 2
- 235000013312 flour Nutrition 0.000 description 2
- 238000004811 liquid chromatography Methods 0.000 description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 1
- 235000019542 Cured Meats Nutrition 0.000 description 1
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 238000000692 Student's t-test Methods 0.000 description 1
- 238000007605 air drying Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 235000015895 biscuits Nutrition 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 235000013373 food additive Nutrition 0.000 description 1
- 239000002778 food additive Substances 0.000 description 1
- 235000019253 formic acid Nutrition 0.000 description 1
- 239000004519 grease Substances 0.000 description 1
- 238000004128 high performance liquid chromatography Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 235000020986 nuts and seeds Nutrition 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 238000004513 sizing Methods 0.000 description 1
- 238000013097 stability assessment Methods 0.000 description 1
- 239000011550 stock solution Substances 0.000 description 1
- 238000012353 t test Methods 0.000 description 1
- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 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
- G01N30/04—Preparation or injection of sample to be analysed
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N2001/2893—Preparing calibration standards
Abstract
The invention relates to a preparation method of a stable tert-butyl hydroquinone standard solution. The method comprises the steps of firstly introducing nitrogen into a used solvent to remove oxygen, illuminating in a darkroom by using a sodium lamp, then weighing a certain amount of beta-mercaptoethanol in a glove box by using an electronic balance with the sensing quantity of 0.00001g, dissolving the beta-mercaptoethanol in the oxygen-removed solvent, weighing tert-butylhydroquinone with the corresponding mass, completely dissolving the tert-butylhydroquinone in the solvent, and fixing the volume by using a volumetric flask qualified for verification after keeping the temperature constant; and finally, filling the standard solution into a glass ampoule bottle in a glove box, and quickly sealing by fusing after taking out the glove box. The tert-butyl hydroquinone standard solution prepared by the method has better stability, solves the problem of oxidation of the tert-butyl hydroquinone standard solution caused by oxygen in the air, and has higher accuracy in the detection process.
Description
Technical Field
The invention belongs to the field of preparation of food detection standard substances, and particularly relates to a preparation method of a tert-butyl hydroquinone standard solution.
Background
Tert-butyl hydroquinone is a fat-soluble antioxidant, and is specified in GB 2760 plus 2011 national standard food additive use Standard for food safety in China: the tert-butyl hydroquinone can be used for fat, oil and emulsified fat products, fat and oil which are basically free of water, cooked nuts and seeds, nut and seed cans, fried flour products, instant rice flour products, moon cakes, biscuits, bakery stuffing, surface sizing, cured meat products, air drying, pressing dry aquatic products and puffed foods, and the maximum using amount of the tert-butyl hydroquinone is 0.2g/kg (calculated by the content of the oil).
A plurality of national standards such as 9 types of antioxidants in GB 5009.32-2016 food safety national standard food, high performance liquid chromatography for measuring antioxidants in SN/T1050 & 2014 export grease, and measurement of a plurality of antioxidants in SN/T3849 & 2014 export food relate to the measurement of the antioxidants in a plurality of foods including tert-butyl hydroquinone. The detection needs the standard solution of the tert-butylhydroquinone, but the standard solution of the tert-butylhydroquinone is easy to oxidize when being prepared. The concentration of the standard stock solution is reduced, so that the concentration of the detection sample is higher, and the detection result is influenced.
Therefore, the preparation of the stable tert-butyl hydroquinone standard solution is important for accurately detecting the content of the antioxidant in the food.
Disclosure of Invention
The invention provides a preparation method of a tert-butylhydroquinone standard solution, aiming at solving the problem of instability of the tert-butylhydroquinone standard solution in the prior art. In the process of preparing the tert-butyl hydroquinone standard solution, the purpose of avoiding light and oxygen is achieved, and the beta-mercaptoethanol is added to improve the stability of the tert-butyl hydroquinone standard solution, so that the concentration value of the prepared tert-butyl hydroquinone standard solution is closer to a theoretical value, and the effective period of the standard solution is prolonged.
In order to solve the technical problems, the invention is realized by the following technical scheme:
the preparation method of the tert-butyl hydroquinone standard solution comprises the following steps:
1) introducing nitrogen into the solvent to remove oxygen to obtain an oxygen-removed solvent;
2) under the environment of a darkroom sodium lamp, required tert-butyl hydroquinone and beta-mercapto ethanol are weighed in a glove box by a high-precision electronic balance, and the mass is accurate to 0.00001 g; wherein the mass of the required standard substance tert-butyl hydroquinone and the volume of the solvent are determined according to the determination of tert-butyl hydroquinoneConcentration C of phenol Standard solution0And volume V0Obtained after calculation;
3) dissolving tert-butyl hydroquinone and beta-mercaptoethanol weighed in the step 2) completely by using the deoxygenated solvent obtained in the step 1), and fixing the volume after keeping the temperature to obtain a tert-butyl hydroquinone standard solution;
4) measuring the concentration value of the tertiary butyl hydroquinone standard solution obtained in the step 3), measuring in parallel for three times, and taking the average value C of the concentration1And will be in the range of measurement uncertainty1The detection concentration of the tertiary butyl hydroquinone standard solution is used;
5) filling the tert-butyl hydroquinone standard solution obtained in the step 3) into a glass ampoule bottle in a glove box, taking out and then quickly sealing by fusing.
Further, in the preparation method of the tert-butyl hydroquinone standard solution, the solvent in the step 1) is methanol, ethanol or acetonitrile, and the three solvents are used in national standards and do not react with tert-butyl hydroquinone.
Further, in the preparation method of the tert-butyl hydroquinone standard solution, in the step 1), nitrogen is introduced into the solvent to remove oxygen, and the nitrogen introduction time is 30-40 min.
Further, in the preparation method of the tert-butylhydroquinone standard solution, in the step 2), the weight amount of the beta-mercaptoethanol is 5% -15% of that of the tert-butylhydroquinone.
Further, in the preparation method of the tert-butyl hydroquinone standard solution, the concentration value of the tert-butyl hydroquinone standard solution in the step 4) is qualitatively and quantitatively detected by using a high performance liquid chromatograph-diode array detector.
Further, the preparation method of the tert-butyl hydroquinone standard solution as described above, step 4) and the measurement uncertainty range are 0.98C0-1.02C0。
After the technical scheme is adopted, the invention has the beneficial effects that: the tert-butyl hydroquinone standard solution prepared by the method uses an oxygen-removing solvent, avoids oxygen and light during preparation, and greatly improves the stability of the product by adding beta-mercaptoethanol, so that the concentration of the product is closer to a theoretical value, and the detection result is more accurate and reliable.
Drawings
FIG. 1 is a flow chart of a preparation method of a tert-butylhydroquinone standard solution
FIG. 2 is a high performance liquid chromatogram of tert-butylhydroquinone in acetonitrile
FIG. 3 is a trend chart of transportation stability of a standard solution of tert-butylhydroquinone in acetonitrile
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below. It will be clear that the described embodiments are only illustrative of the present invention and in no way should be taken as limiting the invention and its applications or uses. 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.
The experimental process of the invention is as follows:
firstly, according to the solvent, volume and concentration information of the tertiary butyl hydroquinone standard solution required by the instruction, selecting the solvent, the tertiary butyl hydroquinone and the beta-mercaptoethanol which correspond to enough using amount, and requiring that all raw materials have a valid raw material certificate to prove the traceability of the raw materials. Then preparing corresponding weighing appliances such as volumetric flasks, beakers, rubber head droppers, weighing boats, weighing spoons and the like.
The solvent is used after nitrogen is introduced to remove oxygen, and the oxygen-removed solvent is obtained.
And calculating the consumption of the required raw materials according to the concentration value and the preparation volume, and completing the preparation of the standard solution in a glove box.
In the glove box, the standard solution is subpackaged into the ampoule bottle, and the ampoule bottle is quickly sealed by melting after being taken out from the glove box.
The present invention will be further described with reference to specific examples.
Example 1
The present invention will be described in detail below with reference to a standard solution of t-butylhydroquinone in acetonitrile at a concentration of 1000. mu.g/mL.
(1) Solution preparation: first, the acetonitrile solvent used was deaerated for 30min by introducing nitrogen gas using a nitrogen blower. The deoxygenated acetonitrile, the tert-butyl hydroquinone raw material, the beta-mercapto acetonitrile raw material and the prepared weighing tool are transferred into a glove box together. In a glove box, about 5mg of beta-mercaptoacetonitrile is weighed out first, and the weighed beta-mercaptoacetonitrile is added into a 100mL volumetric flask and is fully dissolved by deoxygenated acetonitrile. 100mg of tert-butylhydroquinone was weighed out again, and dissolved in a volumetric flask with deoxygenated acetonitrile. And after the temperature of the volumetric flask is stabilized to room temperature, filling the volume of the volumetric flask to 100mL by using deoxygenated acetonitrile, filling the standard solution into a 2mL glass ampoule bottle, and sealing the opening of the ampoule bottle by using a sealing film. And (4) transferring the ampoule bottle out of the glove box, and quickly sealing by fusing to obtain the standard solution of the tert-butyl hydroquinone in the acetonitrile.
(2) And (3) concentration detection: and qualitatively and quantitatively detecting the prepared tert-butyl hydroquinone standard solution in the acetonitrile by using a high performance liquid chromatograph-diode array detector.
The detection parameters are as follows:
a detector: DAD detector, chromatography column: c18, mobile phase: a0.1% formic acid aqueous solution, B acetonitrile, detection wavelength: 294 nm.
The tertiary butyl hydroquinone sample in the acetonitrile is detected for three times, and the test result is shown in the table 1:
TABLE 1 determination of the concentration of tert-butylhydroquinone in acetonitrile
According to the average value C of the detected concentration1The uncertainty range of the standard solution with 1007.02 mu g/mL and a concentration value of 1000 mu g/mL is 980-1020 mu g/mL, and the average value is in the uncertainty range of measurement and meets the experimental requirements.
Uniformity test
According to the general principle and statistical principle of standard substance fixed value of JJF1343-2012, when the number of sample subpackaging units is less than or equal to 200, the number of extraction units is not less than 11. The sampling rule adopts: the first and last 1 are divided into 1, and 9 are randomly extracted in the middle process, 11 are extracted, and analyzed by confirmed liquid chromatography, and each is measured 3 times.
The homogeneity test of the solution standard substance developed at this time adopts a one-factor variance analysis method. The results of the uniformity test are shown in table 2.
TABLE 2 results of homogeneity test of standard solutions
And (4) conclusion: the uniformity test result shows that: there was no significant difference in variance between groups, F (10,22) > F, so that the standard substance could be judged to be uniform.
Stability test
According to the general principle and statistical principle of standard substance valuation of JJF1343-2012, a classic stability assessment scheme is adopted in the study.
The stability test was analyzed by liquid chromatography.
And (4) testing the transportation stability: the solution was stored at 50 ℃ for 12 days, randomly sampled 1 sample per day for different periods (0, 1, 3, 5, 7, 12 days), and the measurements were repeated 3 times, and the average value was taken as the monitoring result. The concentration is plotted against time, and whether the concentration is stable or not is judged by the slope. Table 3 shows the transportation stability test results.
Table 3 transportation stability test results for standard solutions
And (4) conclusion: as can be seen from the trend graph and by the t-test method,
the slope is not obvious, the results are randomly distributed, and no obvious single-direction rising or falling trend is seen, so that the standard substance can be stably stored for 12 days at the temperature of 50 ℃, and the value can be kept stable in the transportation process.
Example 2
Preparation of a standard solution of tert-butylhydroquinone in ethanol: introducing nitrogen into the ethanol solvent for 40min, and preparing a standard solution in a glove box under a sodium lamp. Weighing about 7.5mg of beta-mercaptoethanol, fully dissolving in deoxygenated ethanol, accurately weighing 50mg of pure tert-butylhydroquinone, and fully dissolving in deoxygenated ethanol. After the volumetric flask is cooled to room temperature, the volume is determined to 50ml, the volumetric flask is fully shaken up, the volumetric flask is subpackaged in a 2ml ampoule bottle, and the opening of the ampoule bottle is sealed by a sealing film. And taking the split ampoule bottles out of the glove box, and sealing by fusing at a constant speed to obtain a standard solution of tert-butylhydroquinone in ethanol with the concentration of 1000 mu g/mL.
Example 3
Preparation of a standard solution of tert-butylhydroquinone in methanol: introducing nitrogen into the methanol solvent for 40min, and preparing a standard solution in a glove box under a sodium lamp. Weighing about 1mg of beta-mercapto methanol, fully dissolving in deoxygenated methanol, accurately weighing 10mg of tert-butyl hydroquinone pure product, and fully dissolving in deoxygenated methanol. After the volumetric flask is cooled to room temperature, the volume is determined to be 100ml, the volumetric flask is fully shaken up, the volumetric flask is subpackaged in a 2ml ampoule bottle, and the opening of the ampoule bottle is sealed by a sealing film. And taking the split ampoule bottles out of the glove box, and sealing by fusing at a constant speed to obtain a standard solution of tert-butylhydroquinone in methanol with the concentration of 100 mu g/mL.
According to the invention, the tert-butyl hydroquinone standard solution is prepared in a manner of avoiding light and oxygen and adding beta-mercaptoethanol, so that the problem of poor stability caused by oxidation of tert-butyl hydroquinone can be effectively avoided, and the detection accuracy of tert-butyl hydroquinone is improved.
The above description is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, several modifications and variations can be made without departing from the technical principle of the present invention, and these modifications and variations should also be regarded as the protection scope of the present invention.
Claims (6)
1. The preparation method of the tert-butyl hydroquinone standard solution is characterized by comprising the following steps of:
1) introducing nitrogen into the solvent to remove oxygen to obtain an oxygen-removed solvent;
2) weighing required tert-butyl hydroquinone and beta-mercapto ethanol by using a high-precision electronic balance in a glove box under the environment of a darkroom sodium lamp, wherein the mass is accurate to 0.00001 g; wherein the mass of the required standard substance tert-butylhydroquinone and the volume of the solvent are determined according to the concentration C of the standard solution of tert-butylhydroquinone0And volume V0Obtained after calculation;
3) dissolving tert-butyl hydroquinone and beta-mercaptoethanol weighed in the step 2) completely by using the deoxygenated solvent obtained in the step 1), and fixing the volume after keeping the temperature to obtain a tert-butyl hydroquinone standard solution;
4) measuring the concentration value of the tertiary butyl hydroquinone standard solution obtained in the step 3), measuring in parallel for three times, and taking the average value C of the concentration1And will be in the range of measurement uncertainty1The detection concentration of the tertiary butyl hydroquinone standard solution is used;
5) filling the tert-butyl hydroquinone standard solution obtained in the step 3) into a glass ampoule bottle in a glove box, taking out and then quickly sealing by fusing.
2. The method for preparing a tert-butylhydroquinone standard solution according to claim 1, wherein the solvent in step 1) is methanol, ethanol or acetonitrile.
3. The method for preparing a tert-butylhydroquinone standard solution according to claim 1, wherein in step 1), nitrogen is introduced into the solvent to remove oxygen, wherein the nitrogen introduction time is 30-40 min.
4. The method for preparing a tert-butylhydroquinone standard solution according to claim 1, wherein the weight of the beta-mercaptoethanol in step 2) is 5% -15% of that of tert-butylhydroquinone.
5. The method for preparing a tert-butylhydroquinone standard solution according to claim 1, wherein the concentration value of the tert-butylhydroquinone standard solution in the step 4) is qualitatively and quantitatively detected by using a high performance liquid chromatograph-diode array detector.
6. The method for preparing a tert-butylhydroquinone standard solution according to claim 1, wherein the uncertainty range of the measurement in step 4) is 0.98C0-1.02C0。
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4376118A (en) * | 1980-10-06 | 1983-03-08 | Miles Laboratories, Inc. | Stable nonaqueous solution of tetracycline salt |
| US5098603A (en) * | 1990-01-16 | 1992-03-24 | Eastman Kodak Company | Stabilized phenol solution |
| CN106622021A (en) * | 2016-11-24 | 2017-05-10 | 广东省食品工业研究所 | A method of preparing granular tert-butylhydroquinone |
| CN110988209A (en) * | 2019-12-25 | 2020-04-10 | 山东英盛生物技术有限公司 | LC-MS/MS detection method and pretreatment kit for catecholamine |
| CN112844217A (en) * | 2021-01-15 | 2021-05-28 | 坛墨质检科技股份有限公司 | Preparation method of dicofol standard solution |
-
2022
- 2022-01-26 CN CN202210093127.7A patent/CN114428140A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4376118A (en) * | 1980-10-06 | 1983-03-08 | Miles Laboratories, Inc. | Stable nonaqueous solution of tetracycline salt |
| US5098603A (en) * | 1990-01-16 | 1992-03-24 | Eastman Kodak Company | Stabilized phenol solution |
| CN106622021A (en) * | 2016-11-24 | 2017-05-10 | 广东省食品工业研究所 | A method of preparing granular tert-butylhydroquinone |
| CN110988209A (en) * | 2019-12-25 | 2020-04-10 | 山东英盛生物技术有限公司 | LC-MS/MS detection method and pretreatment kit for catecholamine |
| CN112844217A (en) * | 2021-01-15 | 2021-05-28 | 坛墨质检科技股份有限公司 | Preparation method of dicofol standard solution |
Non-Patent Citations (2)
| Title |
|---|
| 卞晓洁 等: "复方醋酸棉酚片在女性健康志愿者体内的生物等效性研究", 《中国新药杂志》 * |
| 赵慧男 等: "高效液相色谱法分析植物油中9种抗氧化剂", 《色谱》 * |
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