CN101034086A - 磷酸肌酸二钠盐中杂质的检测方法 - Google Patents
磷酸肌酸二钠盐中杂质的检测方法 Download PDFInfo
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- CN101034086A CN101034086A CN 200710038837 CN200710038837A CN101034086A CN 101034086 A CN101034086 A CN 101034086A CN 200710038837 CN200710038837 CN 200710038837 CN 200710038837 A CN200710038837 A CN 200710038837A CN 101034086 A CN101034086 A CN 101034086A
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- liquid chromatography
- creatine phosphate
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- DRBBFCLWYRJSJZ-UHFFFAOYSA-N N-phosphocreatine Chemical compound OC(=O)CN(C)C(=N)NP(O)(O)=O DRBBFCLWYRJSJZ-UHFFFAOYSA-N 0.000 title claims abstract description 83
- 239000012535 impurity Substances 0.000 title claims abstract description 30
- 238000000034 method Methods 0.000 title claims abstract description 29
- QXNVGIXVLWOKEQ-UHFFFAOYSA-N Disodium Chemical compound [Na][Na] QXNVGIXVLWOKEQ-UHFFFAOYSA-N 0.000 title claims description 36
- 238000004811 liquid chromatography Methods 0.000 claims abstract description 14
- CVSVTCORWBXHQV-UHFFFAOYSA-N creatine Chemical compound NC(=[NH2+])N(C)CC([O-])=O CVSVTCORWBXHQV-UHFFFAOYSA-N 0.000 claims description 42
- DDRJAANPRJIHGJ-UHFFFAOYSA-N creatinine Chemical compound CN1CC(=O)NC1=N DDRJAANPRJIHGJ-UHFFFAOYSA-N 0.000 claims description 42
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 34
- 229960003624 creatine Drugs 0.000 claims description 21
- 239000006046 creatine Substances 0.000 claims description 21
- 229940109239 creatinine Drugs 0.000 claims description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 19
- 239000000243 solution Substances 0.000 claims description 18
- BNIILDVGGAEEIG-UHFFFAOYSA-L disodium hydrogen phosphate Chemical compound [Na+].[Na+].OP([O-])([O-])=O BNIILDVGGAEEIG-UHFFFAOYSA-L 0.000 claims description 17
- 229910000397 disodium phosphate Inorganic materials 0.000 claims description 17
- 235000019800 disodium phosphate Nutrition 0.000 claims description 17
- 239000011780 sodium chloride Substances 0.000 claims description 17
- 239000013558 reference substance Substances 0.000 claims description 16
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 15
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 15
- 239000012071 phase Substances 0.000 claims description 15
- 238000012360 testing method Methods 0.000 claims description 11
- 238000000105 evaporative light scattering detection Methods 0.000 claims description 10
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 10
- 238000001514 detection method Methods 0.000 claims description 8
- 229910052816 inorganic phosphate Inorganic materials 0.000 claims description 8
- 239000012074 organic phase Substances 0.000 claims description 7
- DPBLXKKOBLCELK-UHFFFAOYSA-N pentan-1-amine Chemical compound CCCCCN DPBLXKKOBLCELK-UHFFFAOYSA-N 0.000 claims description 7
- 239000007864 aqueous solution Substances 0.000 claims description 6
- 238000000889 atomisation Methods 0.000 claims description 6
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 5
- 235000019253 formic acid Nutrition 0.000 claims description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- 235000014121 butter Nutrition 0.000 claims description 4
- 238000002360 preparation method Methods 0.000 claims description 3
- 239000007789 gas Substances 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims 1
- 238000003908 quality control method Methods 0.000 abstract description 2
- 238000000149 argon plasma sintering Methods 0.000 abstract 1
- 238000001704 evaporation Methods 0.000 abstract 1
- 230000008020 evaporation Effects 0.000 abstract 1
- 230000035945 sensitivity Effects 0.000 abstract 1
- 238000010998 test method Methods 0.000 abstract 1
- 229960002668 sodium chloride Drugs 0.000 description 9
- 239000003814 drug Substances 0.000 description 7
- 239000000126 substance Substances 0.000 description 7
- 238000004128 high performance liquid chromatography Methods 0.000 description 6
- 229910019142 PO4 Inorganic materials 0.000 description 5
- 238000007689 inspection Methods 0.000 description 5
- 239000010452 phosphate Substances 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 4
- 239000003153 chemical reaction reagent Substances 0.000 description 4
- 229940079593 drug Drugs 0.000 description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 4
- 238000000926 separation method Methods 0.000 description 4
- 230000033228 biological regulation Effects 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 229950007002 phosphocreatine Drugs 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 230000005526 G1 to G0 transition Effects 0.000 description 2
- 238000005481 NMR spectroscopy Methods 0.000 description 2
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- 239000012153 distilled water Substances 0.000 description 2
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- 238000002309 gasification Methods 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- 238000001474 liquid chromatography-evaporative light scattering detection Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 230000002107 myocardial effect Effects 0.000 description 2
- YTJSFYQNRXLOIC-UHFFFAOYSA-N octadecylsilane Chemical compound CCCCCCCCCCCCCCCCCC[SiH3] YTJSFYQNRXLOIC-UHFFFAOYSA-N 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 230000001988 toxicity Effects 0.000 description 2
- 231100000419 toxicity Toxicity 0.000 description 2
- 241000370738 Chlorion Species 0.000 description 1
- 206010019133 Hangover Diseases 0.000 description 1
- 206010019280 Heart failures Diseases 0.000 description 1
- 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 description 1
- 101000878457 Macrocallista nimbosa FMRFamide Proteins 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-L Phosphate ion(2-) Chemical compound OP([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-L 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- RXHSGRQJJBSBPN-UHFFFAOYSA-L [Na+].[Na+].Cl.OP([O-])([O-])=O Chemical compound [Na+].[Na+].Cl.OP([O-])([O-])=O RXHSGRQJJBSBPN-UHFFFAOYSA-L 0.000 description 1
- 238000000862 absorption spectrum Methods 0.000 description 1
- XNEIDKOERCQYEG-UHFFFAOYSA-N acetonitrile;pentan-1-amine Chemical compound CC#N.CCCCCN XNEIDKOERCQYEG-UHFFFAOYSA-N 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003293 cardioprotective effect Effects 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
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- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001952 enzyme assay Methods 0.000 description 1
- 238000004190 ion pair chromatography Methods 0.000 description 1
- 238000010829 isocratic elution Methods 0.000 description 1
- 238000012417 linear regression Methods 0.000 description 1
- 230000004060 metabolic process Effects 0.000 description 1
- 208000031225 myocardial ischemia Diseases 0.000 description 1
- 238000005220 pharmaceutical analysis Methods 0.000 description 1
- -1 phosphocreatine acid anhydride Chemical class 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 239000003223 protective agent Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000011003 system suitability test Methods 0.000 description 1
- 238000000825 ultraviolet detection Methods 0.000 description 1
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Abstract
Description
名称 | 加入量(μg/ml) | 实测量(μg/ml) | 回收率(%) |
肌酸 | 88.3 | 85.0 | 96.29 |
99.9 | 98.2 | 98.32 | |
120.1 | 118.5 | 98.67 | |
肌酐 | 80.1 | 78.1 | 97.50 |
100.4 | 98.5 | 98.11 | |
120.4 | 118.1 | 98.09 | |
氯化钠 | 85.0 | 83.8 | 98.53 |
103.2 | 102.2 | 98.99 | |
121.6 | 121.5 | 99.95 | |
磷酸氢二钠 | 79.8 | 78.9 | 98.9 |
100.2 | 99.5 | 99.33 | |
120.1 | 119.6 | 99.59 |
肌酸 | 肌酐 | 氯化钠 | 磷酸氢二钠 | ||||
浓度μg/ml | 峰面积 | 浓度μg/ml | 峰面积 | 浓度μg/ml | 峰面积 | 浓度μg/ml | 峰面积 |
43.70 | 7682 | 24.75 | 4376.4 | 30.35 | 212517 | 39.61 | 73355 |
87.39 | 23338 | 49.50 | 15145.7 | 60.71 | 438265 | 79.22 | 172760 |
174.78 | 58604 | 99.00 | 38040.9 | 121.42 | 890342 | 158.44 | 403308 |
349.57 | 134607 | 198.00 | 83583.5 | 242.84 | 1732325 | 198.05 | 504554 |
524.35 | 209554 | 396.00 | 183368.2 | 607.09 | 4552511 | 396.09 | 1098584 |
r=0.999802 | r=0.999694 | r=0.999811 | r=0.999674 |
名称 | 最小检测限(ng) |
肌酸 | 177.2 |
肌酐 | 161.2 |
无机氯化物(以氯化钠计) | 138.0 |
无机磷酸盐(以磷酸氢二钠计) | 316.9 |
Claims (9)
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CN200710038837A CN101034086B (zh) | 2007-03-30 | 2007-03-30 | 磷酸肌酸二钠盐中杂质的检测方法 |
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CN200710038837A CN101034086B (zh) | 2007-03-30 | 2007-03-30 | 磷酸肌酸二钠盐中杂质的检测方法 |
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CN101034086A true CN101034086A (zh) | 2007-09-12 |
CN101034086B CN101034086B (zh) | 2010-05-19 |
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103760267A (zh) * | 2014-01-16 | 2014-04-30 | 中山百灵生物技术有限公司 | 磷酸肌酸钠二钠盐含量及杂质的高效液相色谱检测方法 |
CN105259286A (zh) * | 2015-10-26 | 2016-01-20 | 上海华拓医药科技发展有限公司 | 磷酸肌酸二钠盐中杂质化合物的高效液相色谱检测方法 |
CN107796883A (zh) * | 2016-09-05 | 2018-03-13 | 上海中医药大学附属龙华医院 | 快速检测组织或者线虫中ATP、ADP、AMP、CP以及creatine含量的方法 |
CN112816609A (zh) * | 2019-11-16 | 2021-05-18 | 重庆圣华曦药业股份有限公司 | 一种在制剂生产过程中检测磷酸肌酸钠残留的方法 |
-
2007
- 2007-03-30 CN CN200710038837A patent/CN101034086B/zh not_active Expired - Fee Related
Cited By (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103760267A (zh) * | 2014-01-16 | 2014-04-30 | 中山百灵生物技术有限公司 | 磷酸肌酸钠二钠盐含量及杂质的高效液相色谱检测方法 |
CN103760267B (zh) * | 2014-01-16 | 2015-05-27 | 中山百灵生物技术有限公司 | 磷酸肌酸二钠盐含量及杂质的高效液相色谱检测方法 |
CN105259286A (zh) * | 2015-10-26 | 2016-01-20 | 上海华拓医药科技发展有限公司 | 磷酸肌酸二钠盐中杂质化合物的高效液相色谱检测方法 |
CN105259286B (zh) * | 2015-10-26 | 2017-03-29 | 上海华拓医药科技发展有限公司 | 磷酸肌酸二钠盐中杂质化合物的高效液相色谱检测方法 |
CN107796883A (zh) * | 2016-09-05 | 2018-03-13 | 上海中医药大学附属龙华医院 | 快速检测组织或者线虫中ATP、ADP、AMP、CP以及creatine含量的方法 |
CN112816609A (zh) * | 2019-11-16 | 2021-05-18 | 重庆圣华曦药业股份有限公司 | 一种在制剂生产过程中检测磷酸肌酸钠残留的方法 |
CN112816609B (zh) * | 2019-11-16 | 2024-04-02 | 重庆圣华曦药业股份有限公司 | 一种在制剂生产过程中检测磷酸肌酸钠残留的方法 |
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