CN103487519B - 一种检测药物中多种残留溶媒的方法 - Google Patents
一种检测药物中多种残留溶媒的方法 Download PDFInfo
- Publication number
- CN103487519B CN103487519B CN201310400084.3A CN201310400084A CN103487519B CN 103487519 B CN103487519 B CN 103487519B CN 201310400084 A CN201310400084 A CN 201310400084A CN 103487519 B CN103487519 B CN 103487519B
- Authority
- CN
- China
- Prior art keywords
- solution
- reference substance
- residual solvent
- solvent
- headspace
- 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.)
- Active
Links
- 239000013557 residual solvent Substances 0.000 title claims abstract description 37
- 238000000034 method Methods 0.000 title claims abstract description 35
- 239000003814 drug Substances 0.000 title claims abstract description 19
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 78
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims abstract description 75
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 72
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 69
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims abstract description 69
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims abstract description 66
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims abstract description 66
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims abstract description 44
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000003960 organic solvent Substances 0.000 claims abstract description 18
- 238000001514 detection method Methods 0.000 claims abstract description 10
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 76
- 239000013558 reference substance Substances 0.000 claims description 59
- 238000012360 testing method Methods 0.000 claims description 49
- 238000005070 sampling Methods 0.000 claims description 26
- 239000002904 solvent Substances 0.000 claims description 26
- 238000002360 preparation method Methods 0.000 claims description 25
- 239000000523 sample Substances 0.000 claims description 23
- 229960002727 cefotaxime sodium Drugs 0.000 claims description 13
- AZZMGZXNTDTSME-JUZDKLSSSA-M cefotaxime sodium Chemical compound [Na+].N([C@@H]1C(N2C(=C(COC(C)=O)CS[C@@H]21)C([O-])=O)=O)C(=O)\C(=N/OC)C1=CSC(N)=N1 AZZMGZXNTDTSME-JUZDKLSSSA-M 0.000 claims description 13
- 230000001174 ascending effect Effects 0.000 claims description 12
- 239000012159 carrier gas Substances 0.000 claims description 12
- 239000004205 dimethyl polysiloxane Substances 0.000 claims description 12
- 238000011067 equilibration Methods 0.000 claims description 12
- 239000000834 fixative Substances 0.000 claims description 12
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 12
- -1 polydimethylsiloxane Polymers 0.000 claims description 12
- 238000005259 measurement Methods 0.000 claims description 11
- 238000012417 linear regression Methods 0.000 claims description 10
- 239000007789 gas Substances 0.000 claims description 9
- 238000007789 sealing Methods 0.000 claims description 8
- 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 description 7
- WNDJSEGRKSORAG-UHFFFAOYSA-N [S].OC(=O)CCC(O)=O Chemical compound [S].OC(=O)CCC(O)=O WNDJSEGRKSORAG-UHFFFAOYSA-N 0.000 claims description 7
- MKUXAQIIEYXACX-UHFFFAOYSA-N aciclovir Chemical compound N1C(N)=NC(=O)C2=C1N(COCCO)C=N2 MKUXAQIIEYXACX-UHFFFAOYSA-N 0.000 claims description 7
- 229960004150 aciclovir Drugs 0.000 claims description 7
- WZOZEZRFJCJXNZ-ZBFHGGJFSA-N cefoxitin Chemical compound N([C@]1(OC)C(N2C(=C(COC(N)=O)CS[C@@H]21)C(O)=O)=O)C(=O)CC1=CC=CS1 WZOZEZRFJCJXNZ-ZBFHGGJFSA-N 0.000 claims description 7
- 229960002682 cefoxitin Drugs 0.000 claims description 7
- 229960002260 meropenem Drugs 0.000 claims description 7
- DMJNNHOOLUXYBV-PQTSNVLCSA-N meropenem Chemical compound C=1([C@H](C)[C@@H]2[C@H](C(N2C=1C(O)=O)=O)[C@H](O)C)S[C@@H]1CN[C@H](C(=O)N(C)C)C1 DMJNNHOOLUXYBV-PQTSNVLCSA-N 0.000 claims description 7
- 239000011734 sodium Substances 0.000 claims description 7
- 229910052708 sodium Inorganic materials 0.000 claims description 7
- 239000012488 sample solution Substances 0.000 claims description 6
- KDYFGRWQOYBRFD-UHFFFAOYSA-N Succinic acid Natural products OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 claims 1
- 239000000243 solution Substances 0.000 abstract description 64
- 238000009835 boiling Methods 0.000 abstract description 4
- 238000004817 gas chromatography Methods 0.000 abstract description 4
- 239000000126 substance Substances 0.000 abstract description 4
- 238000002347 injection Methods 0.000 abstract description 3
- 239000007924 injection Substances 0.000 abstract description 3
- 239000000463 material Substances 0.000 abstract description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 10
- 238000004128 high performance liquid chromatography Methods 0.000 description 5
- 238000003988 headspace gas chromatography Methods 0.000 description 4
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- NCFTXMQPRQZFMZ-WERGMSTESA-M Cefoperazone sodium Chemical compound [Na+].O=C1C(=O)N(CC)CCN1C(=O)N[C@H](C=1C=CC(O)=CC=1)C(=O)N[C@@H]1C(=O)N2C(C([O-])=O)=C(CSC=3N(N=NN=3)C)CS[C@@H]21 NCFTXMQPRQZFMZ-WERGMSTESA-M 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- NTIZESTWPVYFNL-UHFFFAOYSA-N Methyl isobutyl ketone Chemical compound CC(C)CC(C)=O NTIZESTWPVYFNL-UHFFFAOYSA-N 0.000 description 2
- UIHCLUNTQKBZGK-UHFFFAOYSA-N Methyl isobutyl ketone Natural products CCC(C)C(C)=O UIHCLUNTQKBZGK-UHFFFAOYSA-N 0.000 description 2
- NKZMPZCWBSWAOX-IBTYICNHSA-M Sulbactam sodium Chemical compound [Na+].O=S1(=O)C(C)(C)[C@H](C([O-])=O)N2C(=O)C[C@H]21 NKZMPZCWBSWAOX-IBTYICNHSA-M 0.000 description 2
- 238000003965 capillary gas chromatography Methods 0.000 description 2
- 229960002417 cefoperazone sodium Drugs 0.000 description 2
- 229960000479 ceftriaxone sodium Drugs 0.000 description 2
- FDRNWTJTHBSPMW-GNXCPKRQSA-L disodium;(6r,7r)-7-[[(2e)-2-(2-amino-1,3-thiazol-4-yl)-2-methoxyiminoacetyl]amino]-3-[(2-methyl-6-oxido-5-oxo-1,2,4-triazin-3-yl)sulfanylmethyl]-8-oxo-5-thia-1-azabicyclo[4.2.0]oct-2-ene-2-carboxylate Chemical compound [Na+].[Na+].S([C@@H]1[C@@H](C(N1C=1C([O-])=O)=O)NC(=O)/C(=N/OC)C=2N=C(N)SC=2)CC=1CSC1=NC(=O)C([O-])=NN1C FDRNWTJTHBSPMW-GNXCPKRQSA-L 0.000 description 2
- 229940079593 drug Drugs 0.000 description 2
- ZXEKIIBDNHEJCQ-UHFFFAOYSA-N isobutanol Chemical compound CC(C)CO ZXEKIIBDNHEJCQ-UHFFFAOYSA-N 0.000 description 2
- 229940043265 methyl isobutyl ketone Drugs 0.000 description 2
- 229960000614 sulbactam sodium Drugs 0.000 description 2
- 208000027418 Wounds and injury Diseases 0.000 description 1
- 239000002671 adjuvant Substances 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000003640 drug residue Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 125000004836 hexamethylene group Chemical group [H]C([H])([*:2])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[*:1] 0.000 description 1
- 208000014674 injury Diseases 0.000 description 1
- WFKAJVHLWXSISD-UHFFFAOYSA-N isobutyramide Chemical compound CC(C)C(N)=O WFKAJVHLWXSISD-UHFFFAOYSA-N 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- BUTPBERGMJVRBM-UHFFFAOYSA-N methanol;methylsulfinylmethane Chemical compound OC.CS(C)=O BUTPBERGMJVRBM-UHFFFAOYSA-N 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 1
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 1
- 238000010926 purge Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
Landscapes
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
Description
Claims (6)
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201310400084.3A CN103487519B (zh) | 2013-09-05 | 2013-09-05 | 一种检测药物中多种残留溶媒的方法 |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201310400084.3A CN103487519B (zh) | 2013-09-05 | 2013-09-05 | 一种检测药物中多种残留溶媒的方法 |
Publications (2)
Publication Number | Publication Date |
---|---|
CN103487519A CN103487519A (zh) | 2014-01-01 |
CN103487519B true CN103487519B (zh) | 2016-06-22 |
Family
ID=49827905
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN201310400084.3A Active CN103487519B (zh) | 2013-09-05 | 2013-09-05 | 一种检测药物中多种残留溶媒的方法 |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN103487519B (zh) |
Families Citing this family (29)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103926359B (zh) * | 2014-03-24 | 2015-10-28 | 上海新华联制药有限公司 | 一种原料药米非司酮中残留溶剂的测定方法 |
CN105203658B (zh) * | 2015-09-16 | 2017-03-15 | 乐普药业股份有限公司 | 一种依折麦布中残留溶剂的检测方法 |
CN109765304A (zh) * | 2017-11-09 | 2019-05-17 | 郑州泰丰制药有限公司 | 一种硫酸氢氯吡格雷片中乙醇残留的检测方法 |
CN110196304A (zh) * | 2018-02-27 | 2019-09-03 | 广州朗圣药业有限公司 | 一种检测盐酸伐地那非原料药中有机溶剂残留量的方法 |
CN108760951B (zh) * | 2018-05-07 | 2021-03-09 | 山东省药学科学院 | 一种检测生物可吸收聚酯膜中多种残留有机溶剂的方法 |
CN108645933B (zh) * | 2018-05-24 | 2020-10-16 | 河北常山生化药业股份有限公司 | 阿哌沙班原料药中残留溶剂的气相色谱检测方法 |
CN108828124A (zh) * | 2018-06-27 | 2018-11-16 | 湖北省宏源药业科技股份有限公司 | 甲硝唑中残留甲酸甲酯和甲醇限度检查方法 |
CN108760934A (zh) * | 2018-07-13 | 2018-11-06 | 江苏力凡胶囊有限公司 | 一种卡拉胶中残留溶剂的测定方法 |
CN109507309A (zh) * | 2018-10-22 | 2019-03-22 | 重庆中邦科技有限公司 | 回收溶剂中三乙胺和异丙醇的气相色谱分析方法 |
CN109507326A (zh) * | 2018-12-24 | 2019-03-22 | 营口康辉石化有限公司 | 一种pbt中四氢呋喃含量的测定方法及其应用 |
CN109709242A (zh) * | 2019-01-31 | 2019-05-03 | 内蒙古通威高纯晶硅有限公司 | 一种检测氯硅烷中二氯甲烷的方法 |
CN109799309A (zh) * | 2019-02-28 | 2019-05-24 | 河北省药品检验研究院(河北省化妆品检验研究中心) | 一种保泰松中残留溶剂的测定方法 |
CN110501434B (zh) * | 2019-08-12 | 2023-02-07 | 广州茂丰药业有限公司 | 一种含叔氨基甲基丙烯酸酯共聚物中残留溶剂、单体和引发剂分解产物的检测方法 |
CN112964813A (zh) * | 2019-12-13 | 2021-06-15 | 金陵药业股份有限公司 | 一种盐酸法舒地尔中有机溶剂残留量的测定方法 |
CN111289676B (zh) * | 2020-01-20 | 2022-08-16 | 南京林业大学 | 一种检测硫酸特布他林原料药中残留叔丁胺的方法 |
CN111198243A (zh) * | 2020-02-13 | 2020-05-26 | 四川科伦药业股份有限公司 | 一种甲硝唑原料药中残留溶剂乙二醇和二甘醇的检测方法 |
CN111751459A (zh) * | 2020-05-27 | 2020-10-09 | 济川药业集团有限公司 | 一种同时检测西他沙星中多种残留溶剂的方法 |
CN111855839A (zh) * | 2020-06-29 | 2020-10-30 | 武汉九州钰民医药科技有限公司 | 一种头孢噻肟钠中三乙胺的检测方法及其应用 |
CN111812234A (zh) * | 2020-06-30 | 2020-10-23 | 武汉九州钰民医药科技有限公司 | 泮托拉唑钠倍半水合物中残留溶剂的检测方法 |
CN112034069A (zh) * | 2020-09-09 | 2020-12-04 | 安徽丰原药业股份有限公司 | 一种检测乳酸钠溶液中甲醇残留的方法 |
CN112067721A (zh) * | 2020-09-16 | 2020-12-11 | 贵州省分析测试研究院 | 一种硫酸中氯甲烷的检测方法 |
CN112505224B (zh) * | 2020-11-30 | 2022-03-29 | 华南理工大学 | 一种糖蜜酒精废液低沸点组分定量测定方法 |
CN112630346B (zh) * | 2020-12-16 | 2022-11-01 | 河北合佳医药科技集团股份有限公司 | 一种伊布替尼中残留溶剂的定量分析方法 |
CN114113372A (zh) * | 2021-11-08 | 2022-03-01 | 拱北海关技术中心 | 天然食用色素残留溶剂检测方法 |
CN114166974B (zh) * | 2021-12-07 | 2024-03-15 | 河北升泰环境检测有限公司 | 一种气相色谱-质谱检测土壤和沉积物中三乙胺的方法 |
CN114236003A (zh) * | 2021-12-15 | 2022-03-25 | 精晶药业股份有限公司 | 一种泛酸钙挥发性杂质的检测方法 |
CN114236002A (zh) * | 2021-12-15 | 2022-03-25 | 精晶药业股份有限公司 | 一种无水碳酸钠挥发性杂质的检测方法 |
CN115420836B (zh) * | 2022-11-08 | 2023-03-24 | 广州国标检验检测有限公司 | 一种药物中残留小分子有机物的检测方法 |
CN116500172B (zh) * | 2023-06-29 | 2023-09-05 | 成都普康唯新生物科技有限公司 | 一种酸性底物中胺类溶剂的检测方法 |
Family Cites Families (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102323353A (zh) * | 2011-08-16 | 2012-01-18 | 上海新先锋药业有限公司 | 一种检测脂质体药物中有机溶剂残留的方法 |
CN103018353B (zh) * | 2012-10-24 | 2014-09-10 | 宜昌人福药业有限责任公司 | 一种原料药福尔可定中残留溶剂的测定方法 |
-
2013
- 2013-09-05 CN CN201310400084.3A patent/CN103487519B/zh active Active
Also Published As
Publication number | Publication date |
---|---|
CN103487519A (zh) | 2014-01-01 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN103487519B (zh) | 一种检测药物中多种残留溶媒的方法 | |
CN103487541B (zh) | 一种同时检测头孢曲松钠中多种残留溶剂的方法 | |
CN104655751B (zh) | 一种检测达泊西汀中有机溶剂残留的方法 | |
CN105203658B (zh) | 一种依折麦布中残留溶剂的检测方法 | |
CN106153749A (zh) | 检验氯苯达诺盐酸盐原料药中残留溶剂的方法 | |
CN109765313A (zh) | 一种非诺贝特胆碱的检测方法 | |
CN106950291A (zh) | 一种盐酸氨溴索注射剂有关物质的检测方法 | |
CN110849980A (zh) | 一种l-丙氨酸异丙酯中对映异构体含量的检测方法 | |
CN109799298B (zh) | 一种吡仑帕奈原料药中有关物质的检测方法 | |
CN106198819B (zh) | 顶空气相色谱法测定西格列汀原料药中残留溶剂的方法 | |
CN113671077A (zh) | 丙烯酰氯及其有关物质检测方法 | |
CN105929045A (zh) | 一种检测苯磺顺阿曲库铵中有机溶剂残留的方法 | |
CN104849388B (zh) | 测定盐酸阿比多尔原料药中有机溶剂残留含量的方法 | |
CN110895264A (zh) | 一种替诺福韦艾拉酚胺中溴乙烷的测定方法 | |
CN103543231A (zh) | 一种盐酸美克洛嗪中氯仿残留量的分离分析方法 | |
CN108872416A (zh) | 一种同时定量检测芥酸酰胺和乙撑双硬脂酰胺的方法 | |
CN107677737A (zh) | 一种检测维a酸中残留氯仿的方法 | |
CN106018617A (zh) | 一种用液相色谱法分离测定盐酸维拉佐酮中2-氯-1-甲基吡啶鎓碘化物含量的方法 | |
CN102636597A (zh) | 顶空气相色谱法测定盐酸四环素原料药中残留溶剂的方法 | |
CN115343399B (zh) | 一种原料药中n-烷基吡咯烷酮残留溶剂的检测方法 | |
CN105628807B (zh) | 一种1‑Boc‑4‑氨基哌啶的质量检测方法 | |
CN111323493A (zh) | 一种泊沙康唑起始物料对映异构体的检测方法 | |
CN108572223A (zh) | 一种测定多肽中活性诱导物质的方法 | |
CN108593796A (zh) | 一种检测原料药奥希替尼中有机残留溶剂的方法 | |
CN108414648A (zh) | 一种利用顶空气相色谱法检测罗库溴铵中残留溶剂的方法 |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
C06 | Publication | ||
PB01 | Publication | ||
CI01 | Correction of invention patent gazette |
Correction item: Second applicant Correct: Liaoning Medya Pharmaceutical Co., Ltd. False: Liaoning Mei Ya pharmaceutcal corporation, Ltd Number: 01 Volume: 30 |
|
CI02 | Correction of invention patent application |
Correction item: Second applicant Correct: Liaoning Medya Pharmaceutical Co., Ltd. False: Liaoning Mei Ya pharmaceutcal corporation, Ltd Number: 01 Page: The title page Volume: 30 |
|
ERR | Gazette correction |
Free format text: CORRECT: THE SECOND APPLICANT; FROM: LIAONING MEIYA PHARMACEUTICAL CO., LTD. TO: LIAONING MEDYA PHARMACEUTICAL CO., LTD. |
|
RECT | Rectification | ||
EXSB | Decision made by sipo to initiate substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
CB02 | Change of applicant information |
Address after: 201209 Chuansha Road, Shanghai, No. 978, No. Applicant after: SHANGHAI PHARMA NEW ASIA PHARMACEUTICAL CO., LTD. Applicant after: Liaoning Medya Pharmaceutical Co., Ltd. Address before: 201209 Chuansha Road, Shanghai, No. 978, No. Applicant before: Shanghai Xinya Pharmaceutical Industry Co., Ltd. Applicant before: Liaoning Medya Pharmaceutical Co., Ltd. |
|
COR | Change of bibliographic data | ||
C14 | Grant of patent or utility model | ||
GR01 | Patent grant | ||
TR01 | Transfer of patent right |
Effective date of registration: 20170316 Address after: 201209 Chuansha Road, Shanghai, No. 978, No. Patentee after: SHANGHAI PHARMA NEW ASIA PHARMACEUTICAL CO., LTD. Address before: 201209 Chuansha Road, Shanghai, No. 978, No. Patentee before: SHANGHAI PHARMA NEW ASIA PHARMACEUTICAL CO., LTD. Patentee before: Liaoning Medya Pharmaceutical Co., Ltd. |
|
TR01 | Transfer of patent right |