CN102928545A - Method for measuring BHT (butylated hydroxytoluene) content in Pranoprofen eye drops - Google Patents
Method for measuring BHT (butylated hydroxytoluene) content in Pranoprofen eye drops Download PDFInfo
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- CN102928545A CN102928545A CN2012104441610A CN201210444161A CN102928545A CN 102928545 A CN102928545 A CN 102928545A CN 2012104441610 A CN2012104441610 A CN 2012104441610A CN 201210444161 A CN201210444161 A CN 201210444161A CN 102928545 A CN102928545 A CN 102928545A
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- Prior art keywords
- bht
- solution
- reference substance
- pranoprofen
- eye drops
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- TVQZAMVBTVNYLA-UHFFFAOYSA-N Pranoprofen Chemical compound C1=CC=C2CC3=CC(C(C(O)=O)C)=CC=C3OC2=N1 TVQZAMVBTVNYLA-UHFFFAOYSA-N 0.000 title claims abstract description 18
- 229960003101 pranoprofen Drugs 0.000 title claims abstract description 18
- 239000003889 eye drop Substances 0.000 title claims abstract description 12
- 229940012356 eye drops Drugs 0.000 title claims abstract description 12
- 238000000034 method Methods 0.000 title claims abstract description 11
- 239000004322 Butylated hydroxytoluene Substances 0.000 title abstract 5
- NLZUEZXRPGMBCV-UHFFFAOYSA-N Butylhydroxytoluene Chemical compound CC1=CC(C(C)(C)C)=C(O)C(C(C)(C)C)=C1 NLZUEZXRPGMBCV-UHFFFAOYSA-N 0.000 title abstract 5
- 229940095259 butylated hydroxytoluene Drugs 0.000 title abstract 5
- 235000010354 butylated hydroxytoluene Nutrition 0.000 title abstract 5
- 239000013558 reference substance Substances 0.000 claims abstract description 15
- 239000000243 solution Substances 0.000 claims description 23
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 21
- 238000012360 testing method Methods 0.000 claims description 12
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 8
- 238000002360 preparation method Methods 0.000 claims description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- 229960000583 acetic acid Drugs 0.000 claims description 4
- 239000012362 glacial acetic acid Substances 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 238000001514 detection method Methods 0.000 claims description 3
- 238000010812 external standard method Methods 0.000 claims description 3
- 239000000945 filler Substances 0.000 claims description 3
- YTJSFYQNRXLOIC-UHFFFAOYSA-N octadecylsilane Chemical compound CCCCCCCCCCCCCCCCCC[SiH3] YTJSFYQNRXLOIC-UHFFFAOYSA-N 0.000 claims description 3
- 239000000377 silicon dioxide Substances 0.000 claims description 3
- 238000011003 system suitability test Methods 0.000 claims description 3
- 238000003556 assay Methods 0.000 claims description 2
- PBCJIPOGFJYBJE-UHFFFAOYSA-N acetonitrile;hydrate Chemical compound O.CC#N PBCJIPOGFJYBJE-UHFFFAOYSA-N 0.000 claims 1
- GBMDVOWEEQVZKZ-UHFFFAOYSA-N methanol;hydrate Chemical compound O.OC GBMDVOWEEQVZKZ-UHFFFAOYSA-N 0.000 abstract description 2
- 238000004007 reversed phase HPLC Methods 0.000 abstract 1
- 239000000523 sample Substances 0.000 description 6
- 239000000126 substance Substances 0.000 description 3
- 239000003963 antioxidant agent Substances 0.000 description 2
- 230000003078 antioxidant effect Effects 0.000 description 2
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000004128 high performance liquid chromatography Methods 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 206010010741 Conjunctivitis Diseases 0.000 description 1
- 101100256637 Drosophila melanogaster senju gene Proteins 0.000 description 1
- 206010061218 Inflammation Diseases 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 208000010217 blepharitis Diseases 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000006196 drop Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000004054 inflammatory process Effects 0.000 description 1
- 206010023332 keratitis Diseases 0.000 description 1
- 239000002075 main ingredient Substances 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 239000000041 non-steroidal anti-inflammatory agent Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 235000019260 propionic acid Nutrition 0.000 description 1
- 239000008213 purified water Substances 0.000 description 1
- 238000003908 quality control method Methods 0.000 description 1
- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 description 1
- 238000004366 reverse phase liquid chromatography Methods 0.000 description 1
- 239000012488 sample solution Substances 0.000 description 1
- 230000003637 steroidlike Effects 0.000 description 1
- 238000002636 symptomatic treatment Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
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- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention discloses a method for measuring BHT (butylated hydroxytoluene) content in Pranoprofen eye drops. The method is a reversed phase high-performance liquid chromatography utilizing pure BHT as a reference substance and methanol-water as a moving phase. Compared with the prior art, the method is easy, accurate and high in specificity.
Description
Technical field:
The present invention relates to the content assaying method of BHT in a kind of pranoprofen eye drops, belong to drug quality control technology field.
Background technology:
Pranoprofen (Pranoprofen), chemical name: (RS)-and 2-(10-hydrogen-9-Evil-1-naphthazine-6-yl) propionic acid, chemical structural formula:
Molecular formula: C
15H
13NO
3, 255.27
Pranoprofen is the non-steroidal anti-inflammatory analgesics thing of welfide company (former Ji Fu Pharmaceutical Co., Ltd, the pharmacy of existing Mitsubishi) exploitation.Senju Pharma Co., Ltd is developed as eye drops with it, goes on the market in Japan in 1988.The symptomatic treatment that is used for clinically the inflammation of eye section such as blepharitis, conjunctivitis, keratitis, sclerotitis.
BHT, chemical name are 2,6-di-tert-butyl-4-methy phenol, by Bayer A.G's invention, are used as antioxidant in food processing, rubber plastic.
Molecular formula: C
15H
24O, 220.35
Oxidation reaction easily occurs in the main ingredient pranoprofen in the pranoprofen eye drops, generates oxidation product, thus add BHT as antioxidant to keep the stable of preparation, prolong its term of validity.
Summary of the invention:
The object of the present invention is to provide the content assaying method of BHT in a kind of pranoprofen eye drops, it is accurate, easy to measure.
The present invention is achieved through the following technical solutions: the content assaying method of BHT in the pranoprofen eye drops is take the BHT sterling as reference substance, the reversed-phased high performace liquid chromatographic take methanol-water as mobile phase.
It is further characterized in that concrete assay method step is:
(1) chromatographic condition and system suitability test: be filling agent with octadecylsilane chemically bonded silica; Methyl alcohol: water (90: 10) (take the glacial acetic acid adjust pH as 5.2) is mobile phase; Flow velocity is 1.0ml/min; The detection wavelength is 275nm, and sample size is 20 μ L; Theoretical cam curve is calculated by pranoprofen and is not less than 2500;
(2) preparation of reference substance solution: accurate BHT reference substance is an amount of, also quantitatively is diluted to the solution of 50 μ g/ml with the methyl alcohol dissolving, in contrast product solution;
(3) preparation of need testing solution: precision measures sample 5ml and puts in the 10ml volumetric flask, adds mobile phase and is diluted to scale, shakes up, as need testing solution;
(4) measure: get respectively each 20 μ L of reference substance solution and need testing solution and inject high performance liquid chromatograph, the record peak area is pressed the content that external standard method is calculated BHT in the test sample.
Measure the content of BHT in the pranoprofen eye drops with the present invention, owing to adopting reversed phase liquid chromatography to detect, specificity is strong, thereby easy, accurate.
Description of drawings:
Fig. 1 is the chromatogram of reference substance solution of the present invention;
Fig. 2 is the chromatogram of sample solution of the present invention.
Specific implementation method:
Further set forth the present invention below by example, but do not place restrictions on the present invention.
Embodiment 1:
Instrument: the Japanese Shimadzu LC-10AT VP of company high performance liquid chromatograph; The SPD-10A UV-detector; And the HPLC chromatographic work station of analytical instrument outfit;
Chromatographic column: Kromasil 100-5C18 chromatographic column (250mm * 4.6mm);
Reference substance: BHT reference substance (detect through HPLC, purity is 99.1%);
Reagent: purified water, methyl alcohol (chromatographically pure), glacial acetic acid (chromatographically pure);
Chromatographic condition and system suitability test: be filling agent with octadecylsilane chemically bonded silica; Methyl alcohol: water (90: 10) (take the glacial acetic acid adjust pH as 5.2) is mobile phase; Flow velocity is 1.0ml/min; The detection wavelength is 275nm, and sample size is 20 μ L; Theoretical cam curve is calculated by pranoprofen and is not less than 2500;
The preparation of reference substance solution: accurate BHT reference substance is an amount of, also quantitatively is diluted to the solution of 50 μ g/ml with the methyl alcohol dissolving, in contrast product solution;
The preparation of need testing solution: precision measures sample 5ml and puts in the 10ml volumetric flask, adds mobile phase and is diluted to scale, shakes up, as need testing solution;
Measure: get respectively each 20 μ L of reference substance solution and need testing solution and inject high performance liquid chromatograph, the record peak area is pressed the content that external standard method is calculated BHT in the test sample.
The retention time of BHT is 10.32min in the pranoprofen eye drops, and the content of BHT is respectively after measured in three batch samples: 0.03 ‰, 0.04 ‰, 0.04 ‰.
Below disclose the present invention with preferred embodiment, so it is not intended to limiting the invention, and all employings are equal to replaces or technical scheme that the equivalent transformation mode obtains, all drops within protection scope of the present invention.
Claims (2)
1. the content assaying method of BHT in the pranoprofen eye drops is characterized in that take the BHT sterling as reference substance the reversed-phased high performace liquid chromatographic take acetonitrile-water as mobile phase.
2. the content assaying method of BHT in the pranoprofen eye drops according to claim 1 is characterized in that concrete assay method step is:
(1) chromatographic condition and system suitability test: be filling agent with octadecylsilane chemically bonded silica; The volume ratio of methyl alcohol and water is 90: 10, take the glacial acetic acid adjust pH as 5.2 as mobile phase; Flow velocity is 1.0ml/min; The detection wavelength is 245nm, and sample size is 20 μ L; Theoretical cam curve is calculated by pranoprofen and is not less than 2500;
(2) preparation of reference substance solution: accurate BHT reference substance is an amount of, also quantitatively is diluted to the solution of 50 μ g/ml with the methyl alcohol dissolving, in contrast product solution;
(3) preparation of need testing solution: precision measures sample 5ml and puts in the 10ml volumetric flask, adds mobile phase and is diluted to scale, shakes up, as need testing solution;
(4) measure: get respectively each 20 μ L of reference substance solution and need testing solution and inject high performance liquid chromatograph, the record peak area is pressed the content that external standard method is calculated BHT in the test sample.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012104441610A CN102928545A (en) | 2012-11-09 | 2012-11-09 | Method for measuring BHT (butylated hydroxytoluene) content in Pranoprofen eye drops |
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|---|---|---|---|
| CN2012104441610A CN102928545A (en) | 2012-11-09 | 2012-11-09 | Method for measuring BHT (butylated hydroxytoluene) content in Pranoprofen eye drops |
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| CN2012104441610A Pending CN102928545A (en) | 2012-11-09 | 2012-11-09 | Method for measuring BHT (butylated hydroxytoluene) content in Pranoprofen eye drops |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105527357A (en) * | 2016-02-04 | 2016-04-27 | 广东省医疗器械质量监督检验所 | Method for determining antioxidant BHT in insulin glargine injection |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102128886A (en) * | 2010-12-09 | 2011-07-20 | 国药集团化学试剂有限公司 | High performance liquid chromatography method for measuring stabilizer BHT content of tetrahydrofuran |
| CN102175782A (en) * | 2010-12-21 | 2011-09-07 | 上海谱尼测试技术有限公司 | Method for detecting antioxidant in food |
-
2012
- 2012-11-09 CN CN2012104441610A patent/CN102928545A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102128886A (en) * | 2010-12-09 | 2011-07-20 | 国药集团化学试剂有限公司 | High performance liquid chromatography method for measuring stabilizer BHT content of tetrahydrofuran |
| CN102175782A (en) * | 2010-12-21 | 2011-09-07 | 上海谱尼测试技术有限公司 | Method for detecting antioxidant in food |
Non-Patent Citations (10)
| Title |
|---|
| HADJMOHAMMADI M.R. ET AL: "Application of experimental design for extraction of BHA and BHT from edible vegetable oil and their determination using HPLC", 《QSCIENCE CONNECT》 * |
| JOLANA K ET AL: "Determination of synthetic phenolic antioxidants in food by high-performance liquid chromatography", 《JOURNAL OF CHROMATOGRAPHY A》 * |
| 中华人民共和国国家质量监督检验检疫总局: "《中华人民共和国国家标准GB/T 22728-2008》", 31 December 2008 * |
| 何国亮: "高效液相色谱快速测定食品及饲料中抗氧化剂BHT", 《粮油食品科技》 * |
| 商军 等: "高效液相色谱法同时测定饲料中四种抗氧化剂含量", 《上海市畜牧兽医学会2011年学术年会论文集 》 * |
| 张禹华 等: "HPLC法测定普拉洛芬滴眼液中有关物", 《中国科技博览》 * |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105527357A (en) * | 2016-02-04 | 2016-04-27 | 广东省医疗器械质量监督检验所 | Method for determining antioxidant BHT in insulin glargine injection |
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Application publication date: 20130213 |