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美国药典USP40-左氧氟沙星API

美国药典USP40-左氧氟沙星API
美国药典USP40-左氧氟沙星API

USP 40

Official Monographs / Levofloxacin 4831

Acceptance criteria: See Table 1.

Sample solution: 1mg/mL of Levofloxacin in Mobile phase

Chromatographic system

Table 1(See Chromatography ?621?, System Suitability .)Relative Relative Acceptance Mode: LC

Retention Response Criteria,Detector: UV 360 nm

Name

Time

Factor NMT (%)

Column: 4.6-mm × 25-cm; 5-μm packing L1Levodopa related Column temperature: 45°compound A 0.90.830.1Flow rate: 0.8mL/min Injection size: 25μL Levodopa

1.0——System suitability

Levodopa related Sample: Standard solution compound B 2.8

0.83

0.5

Suitability requirements 5,6-Dihydroxy-in-Tailing factor: 0.5–1.5

dole-2-carboxylic Relative standard deviation: NMT 1.0%acid

6.0 2.5

0.1Analysis

0.1Samples: Standard solution and Sample solution

individual Calculate the percentage of levofloxacin (C 18H 20FN 3O 4)—

0.3 total in the portion of Levofloxacin taken:

Unknown impurities 1.0unknown Total impurities

1.1

Result = (r U /r S ) × (C S /C U ) × 100

r U

= peak response of levofloxacin from the Sample

ADDITIONAL REQUIREMENTS

solution

?P ACKAGING AND S TORAGE : Preserve in tight, light-resistant r S = peak response of levofloxacin from the

containers, in a dry place, and prevent exposure to ex-Standard solution

cessive heat.

C S = concentration of USP Levofloxacin RS in the

?USP R EFERENCE S TANDARDS ?11?Standard solution (mg/mL)

USP Levodopa RS

C U = concentration of Levofloxacin in the Sample

USP Levodopa Related Compound A RS solution (mg/mL)

3-(3,4,6-Trihydroxyphenyl)alanine.Acceptance criteria: 98.0%–102.0% on the anhydrous C 9H 11NO 5213.19

basis

USP Levodopa Related Compound B RS 3-Methoxytyrosine.IMPURITIES

C 10H 13NO 4211.22

?R ESIDUE ON I GNITION ?281?: NMT 0.2%. Use a platinum crucible.

Delete the following:

Levofloxacin

??H EAVY M ETALS , Method II ?231?: NMT 10ppm ?(Official 1-Jan-2018)

?O RGANIC I MPURITIES , P ROCEDURE 1

[N OTE —Procedure 1 is recommended if levofloxacin N -ox-ide is a potential organic impurity. Procedure 2 and Pro-cedure 3 are recommended if levofloxacin related com-pound B is a potential organic impurity.]

Solution A, Mobile phase, Sample solution, and Chro-matographic system: Proceed as directed in the C 18H 20FN 3O 4·1/2H 2O 370.38Assay .

7H -Pyrido[1,2,3-de ]-1,4-benzoxazine-6-carboxylic acid,

System suitability solution: 1mg/mL of USP Levoflox-9-fluoro-2,3-dihydro-3-methyl-10-(4-methyl-1-piperazinyl)-acin RS in Mobile phase

7-oxo-hydrate (2:1), (S )-;

Sensitivity solution: 0.3μg/mL of USP Levofloxacin RS (?)-(S )-9-Fluoro-2,3-dihydro-3-methyl-10-(4-methyl-1-piper-in Mobile phase azinyl)-7-oxo-7H -pyrido[1,2,3-de ]-1,4-benzoxazine-6-car-System suitability

boxylic acid, hemihydrate [138199-71-0].Samples: System suitability solution and Sensitivity Anhydrous [100986-85-41].

solution

Suitability requirements

DEFINITION

Relative standard deviation: NMT 1.0%, System suit-Levofloxacin contains NLT 98.0% and NMT 102.0% of ability solution

C 18H 20FN 3O 4, calculated on the anhydrous basis.Signal-to-noise ratio: NLT 10, Sensitivity solution IDENTIFICATION

Analysis

?A . I NFRARED A BSORPTION ?197K ?

Sample: Sample solution

?B . The retention time of the major peak of the Sample Calculate the percentage of each individual impurity in solution corresponds to that of the Standard solution , as the portion of Levofloxacin taken:

obtained in the Assay.Result = (r U /r S ) × (1/F ) × 100

ASSAY

?P ROCEDURE

r U = peak response of each impurity Buffer: 8.5g/L of ammonium acetate, 1.25g/L of cu-r S = peak response of levofloxacin pric sulfate, pentahydrate, and 1.3g/L of L -isoleucine in F = relative response factor (see Table 1)water

Acceptance criteria: See Table 1.

Mobile phase: Methanol and Buffer (3:7)

Standard solution: 1mg/mL of USP Levofloxacin RS in Mobile phase

USP Monographs

4832Levofloxacin / Official Monographs

USP 40

Table 1in methanol from Levofloxacin related compound B stock solution

Relative Relative Acceptance Standard solution: 0.4μg/mL of levofloxacin and

Retention Response Criteria,0.8μg/mL of levofloxacin related compound B in aceto-Name

Time

Factor

NMT (%)

nitrile and water (1:10) from Levofloxacin standard solu-N -Desmethyl tion and Levofloxacin related compound B standard levofloxacin a

0.47 1.00.3solution

Diamine derivative b 0.520.90.3Sample solution: 0.4mg/mL by dissolving the sample Levofloxacin in acetonitrile at about 8% of final volume and diluting N -oxide c

0.63 1.10.3with water to volume. [N OTE —Sonicate if necessary.]Chromatographic system

9-Desfluoro levoflox-(See Chromatography ?621?, System Suitability .)acin d

0.73 1.00.3Mode: LC

Levofloxacin 1.0——Detector: 280 nm

D -Isomer e

1.23 1.00.8Column: 4.0-mm × 15-cm; 3.0-μm packing L1Any unknown Column temperature: 38°—impurity

1.00.1Flow rate: 1.0mL/min Total Impurities

0.5*

Injection size: 10μL a

(S )-9-Fluoro-2,3-dihydro-3-methyl-10-(piperazin-1-yl)-7-oxo-7H -pyrido[1,System suitability

2,3-de ][1,4]benzoxazine-6-carboxylic acid.

Sample: System suitability solution b (S )-9-Fluoro-2,3-dihydro-3-methyl-10-[2-(methylamino)ethylamino]-7-Suitability requirements

oxo-7H -pyrido[1,2,3-de ][1,4]benzoxazine-6-carboxylic acid.

Relative standard deviation: NMT 2.0% for c (S )-4-(6-Carboxy-9-fluoro-2,3-dihydro-3-methyl-7-oxo-7H -pyrido-[1,2,3-levofloxacin de ][1,4]benzoxazine-10-yl)-1-methyl-piperazine-1-oxide.

Analysis

d (S )-2,3-Dihydro-3-methyl-10-(4-methyl-1-piperazinyl)-7-oxo-7H -pyrido[1,Samples: Standard solution and Sampl

e solution

2,3-de ][1,4]benzoxazine-6-carboxylic acid.

Calculate the percentage of levofloxacin related com-e (R )-9-Fluoro-2,3-dihydro-3-methyl-10-(4-methyl-1-piperazinyl)-7-oxo-7H -pyrido[1,2,3-de ][1,4]benzoxazine-6-carboxylic acid.

pound B in the portion of Levofloxacin taken:

*Do not include the D -isomer in the calculation for total impurities.

Result = (r U /r S ) × (C S /C U ) × 100

?O RGANIC I MPURITIES , P ROCEDURE 2

[N OTE —Solutions of levofloxacin are not stable in light;r U

= peak response for levofloxacin related

use amber bottles.]

compound B from the Sample solution

Buffer: Dissolve 3.08g/L of ammonium acetate and r S = peak response for levofloxacin related

8.43g/L of sodium perchlorate monohydrate in https://www.wendangku.net/doc/5013230011.html,pound B from the Standard solution

Adjust with phosphoric acid to a pH of 2.2.C S = concentration of USP Levofloxacin Related

Solution A: Acetonitrile and Buffer (16:84)Compound B RS in the Standard solution Solution B: Acetonitrile, methanol, and Buffer (mg/mL)

(30:20:50)

C U = concentration of Levofloxacin in the Sample

Solution C: 0.4mg/mL of USP Levofloxacin RS by dis-solution (mg/mL)

solving in acetonitrile at about 8% of volume and dilut-Calculate the percentage of other impurities in the ing with water to volume

portion of Levofloxacin taken:

Solution D: 0.05mg/mL of USP Levofloxacin Related Compound A RS in 0.2% ammonium hydroxide in Result = (r U /r S ) × (C S /C U ) × 100

methanol

Mobile phase: See Table 2.

r U

= peak response of any other impurity from the

Sample solution

r S = peak response of levofloxacin from the

Table 2

Standard solution

Time Solution A

Solution B

C S = concentration of USP Levofloxacin RS in the

(min)(%)(%)standard solution (mg/mL)

01000C U = concentration of Levofloxacin in the Sample

solution (mg/mL)

51000Acceptance criteria: See Table 3.

108218154060Table 3

30406030.11000Relative Acceptance Retention Criteria,38

100

Name

Time

NMT (%)

System suitability solution: 0.1mg/mL of USP

Levofloxacin related compound A Levofloxacin RS and 5μg/mL of USP Levofloxacin Re-(N -Desmethyl levofloxacin)a 0.90.20lated Compound A RS in water from Solution C and Levofloxacin

1.0—Solution D

Levofloxacin related compound B b 2.90.13Levofloxacin stock solution: 0.4mg/mL of USP

Any other impurity —0.10Levofloxacin RS. Dissolve USP Levofloxacin RS in aceto-Total impurities

0.50

nitrile at about 8% of final volume, sonicate, and dilute with water to volume.

a

(S )-9-Fluoro-3-methyl-10-(piperazin-1-yl)-7-oxo-2,3-dihydro-7H -pyrido[1,2,3-de ][1,4-benzoxazine-6-carbocylic acid.

Levofloxacin standard solution: 0.02mg/mL of USP b (S )-9,10-Difluoro-3-methyl-7-oxo-2,3-dihydro-7H -pyrido[1,2,3-de ][1,4-Levofloxacin RS in acetonitrile and water (1:10) from benzoxazine-6-carbocylic acid.

Levofloxacin stock solution

Levofloxacin related compound B stock solution:?O RGANIC I MPURITIES (E NANTIOMERIC P URITY), P ROCEDURE 3

0.2mg/mL USP Levofloxacin Related Compound B RS Buffer: 1.32g/L of D -phenylalanine and 0.75g/L of in methanol. [N OTE —Sonicate if necessary.]

copper(II)sulfate pentahydrate in water

Levofloxacin related compound B standard solution:0.04mg/mL USP Levofloxacin Related Compound B RS

U S P M o n o g r a p h s

USP 40Official Monographs / Levofloxacin4833

Mobile phase: Methanol and Buffer (15:85)ASSAY

System suitability solution: 0.01mg/mL of USP Oflox-?P ROCEDURE

acin RS and 0.01mg/mL of USP Levofloxacin RS in[N OTE—Protect the solutions of levofloxacin from light.] water Diluent: Acetonitrile and water (18:82)

Sample solution: 0.08mg/mL in water Mobile phase:Diluent that contains 1mL of trifluoroa-Chromatographic system cetic acid in each 1000mL of solution

(See Chromatography ?621?, System Suitability.)Standard solution: 102.5μg/mL of USP Levofloxacin

Mode: LC RS in Diluent

Detector: 294 nm System suitability solution: 102.5μg/mL each of USP Column: 4.6-mm × 15-cm; 3.5-μm packing L1Levofloxacin RS and USP Levofloxacin Related Com-

Column temperature: 40°pound A RS in Diluent

Flow rate: 0.7mL/min Sample solution: 102.5μg/mL of levofloxacin in Dilu-Injection size: 10μL ent based on the label claim. [N OTE—Mix the solution System suitability well after equilibrating the solution for 4 h at room

Sample:System suitability solution temperature while protected from light.]

[N OTE—The relative retention times for D-ofloxacin and Chromatographic system

levofloxacin are 0.91 and 1.0, respectively.](See Chromatography ?621?, System Suitability.)

Suitability requirements Mode: LC

Resolution: NLT 2.0 between D-ofloxacin (D-isomer)Detector: UV 294 nm

and levofloxacin Column: 4.6-mm × 15-cm; 3.5-μm packing L11 Analysis Column temperature: 30°

Sample: Sample solution Flow rate: 0.7mL/min

Calculate the percentage of D-ofloxacin in the portion Run time: 2.5 times the retention time of the levoflox-of Levofloxacin taken:acin peak

Injection size: 20μL

Result = (r U/r T) × 100System suitability

Samples:Standard solution and System suitability r U= peak response for D-ofloxacin solution

r T= sum of responses of all peaks Suitability requirements

Acceptance criteria: NMT 1.0%Resolution: NLT 1.9 between levofloxacin related

compound A and levofloxacin, System suitability SPECIFIC TESTS solution

?O PTICAL R OTATION, Specific Rotation ?781S?Relative standard deviation: NMT 2.0%, Standard Solvent: Methanol solution

Sample solution: 5mg/mL in Solvent Analysis

Acceptance criteria:?92° to ?106°, at 20°Samples:Standard solution and Sample solution

?W ATER D ETERMINATION, Method Ia?921?: 2.0%–3.0%Calculate the percentage of the labeled amount of

levofloxacin (C18H20FN3O4) in the portion of Oral Solu-

USP Monographs ADDITIONAL REQUIREMENTS

tion taken:

?P ACKAGING AND S TORAGE: Preserve in tight, light-resistant

containers. Store at room temperature.Result = (r

U/r S) × (C S/C U) × 100

?L ABELING: If a procedure for Organic Impurities other than

Procedure 1 is used, then the labeling states with which r

U= peak response from the Sample solution Organic Impurities procedure the article complies.r

S= peak response from the Standard solution

?USP R EFERENCE S TANDARDS?11?C

S= concentration of USP Levofloxacin RS in the USP Levofloxacin RS Standard solution (mg/mL)

USP Levofloxacin Related Compound A RS C

U= nominal concentration of levofloxacin in the (S)-9-Fluoro-3-methyl-10-(piperazin-1-yl)-7-oxo-2,3-Sample solution (mg/mL)

dihydro-7H-pyrido[1,2,3-de][1,4]benzoxazine-6-carbox-Acceptance criteria: 90.0%–110.0%

ylic acid.

C17H18FN3O4 347.34IMPURITIES

USP Levofloxacin Related Compound B RS Organic Impurities

(S)-9,10-Difluoro-3-methyl-7-oxo-2,3-dihydro-7H-pyrido?P ROCEDURE

[1,2,3-de][1,4]benzoxazine-6-carboxylic acid.[N OTE—Protect the solutions of levofloxacin from light.] C13H9F2NO4 281.21Diluent, Mobile phase, Standard solution, System

USP Ofloxacin RS suitability solution, Sample solution, Chromato-

graphic system, and System suitability: Proceed as

directed in the Assay.

Analysis

Samples:Standard solution and Sample solution Levofloxacin Oral Solution Calculate the percentage of each individual impurity in

the portion of Oral Solution taken:

DEFINITION

Result = (r U/r S) × (C S/C U) × (1/F) × 100 Levofloxacin Oral Solution contains NLT 90.0% and NMT

110.0% of the labeled amount of levofloxacin

r U= peak response of each individual impurity

(C18H20FN3O4).

from the Sample solution

r S= peak response of levofloxacin from the IDENTIFICATION

Standard solution

?A. The retention time of the major peak of the Sample

C S= concentration of USP Levofloxacin RS in the

solution corresponds to that of the Standard solution, as

Standard solution (mg/mL) obtained in the Assay.

C U= nominal concentration of levofloxacin in the

Sample solution (mg/mL)

F= relative response factor for each impurity (See

Impurity Table 1)

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usp美国药典结构梳理

USP35-NF-30结构整理 vivi2010-10-02 USP总目录: 1 New Official Text修订文件 加快修订过程包括勘误表,临时修订声明(IRAS),修订公告。勘误表,临时修订声明,修订公告在USP网站上New Official Text部分刊出,勘误表,临时修订公告也会在PF上刊出2front matter前言 药典与处方集增补删减情况,审核人员,辅料收录情况 3凡例

药典, 1标题和修订 2 药典地位和法律认可 3标准复合性 4专论和通则 5 专论组成 6 检验规范和检验方法 7 测试结果 8 术语和定义 9 处方和配药 10 包装存储与标签 4通则 4.1章节列表 4.2一般检查和含量测定(章节编号小于1000)

检查和含量分析的一般要求 检查和含量分析的仪器, 微生物检查,生物检查和含量测定, 化学检查和含量测定, 物理检查和测定 4.3一般信息(章节号大于1000) 5食物补充剂通则 6试剂(试剂,指示剂,溶液等) 7参考表 性状描述和溶解性查询表(按字母顺序) 8食品补充剂各论(字母顺序) 9NF各论(辅料标准) 10 USP各论 11术语 附件:通则的章节中文目录(使用起来比较方便,直接找对应章节号即可)一、通用试验和检定 (1)试验和检定的总要求 1 注射剂 11 参比标准物 (2)试验和检定的装置 16 自动分析方法 21 测温仪 31 容量装置,如容量瓶、移液管、滴定管,各种规格的误差限度

41 砝码和天平 (3)微生物学试验 51 抗菌效力试验 55 生物指示剂:耐受性能试验 61 微生物限度试验 61 非灭菌制品的微生物检查:计数试验 62 非灭菌制品的特定菌检查,如大肠杆菌、金葡菌、沙门氏菌等 71 无菌试验 (4)生物学试验和检定 81 抗生素微生物检定 85 细菌内毒素试验 87 体外生物反应性试验:检查合成橡胶、塑料、高聚物对哺乳类细胞培养的影响 88 体内生物反应性试验:检查上述物质对小鼠、兔iv、ip或肌内植入的影响 91 泛酸钙检定 111 生物检定法的设计和分析 115 右泛醇检定 121 胰岛素检定 141 蛋白质——生物适应试验,用缺蛋白饲料大鼠,观察水解蛋白注射液和氨基酸混合物的作用 151 热原检查法 161 输血、输液器及类似医疗装置的内毒素、热原、无菌检查 171 维生素B12 活性检定 (5)化学试验和检定 A 鉴别试验 181 有机含氮碱的鉴别 191 一般鉴别试验 193 四环素类鉴别 197 分光光度法鉴别试验 201 薄层色谱鉴别试验 B 限量试验

美国药典USP31(921)翻译版(上)

921WATER DETERMINATION水分测定 Many Pharmacopeial articles either are hydrates or contain water in adsorbed form. As a result, the determination of the water content is important in demonstrating compliance with the Pharmacopeial standards. Generally one of the methods given below is called for in the individual monograph, depending upon the nature of the article. In rare cases, a choice is allowed between two methods. When the article contains water of hydration, the Method I (Titrimetric), the Method II (Azeotropic), or the Method III (Gravimetric) is employed, as directed in the individual monograph, and the requirement is given under the heading Water. 很多药典物品要么是水合物,要么含有处于吸附状态的水。因此,测定水分含量对于证实与药典标准的符合性是很重要的。通常,在具体的各论中会根据该物品的性质,要求使用下面若干方法中的一个。偶尔,会允许在2个方法中任选一个。当该物品含有水合状态的水,按照具体各论中的规定,使用方法I(滴定测量法)、方法II(恒沸测量法)、或方法III(重量分析法),这个要求在标题水分项下给出。 The heading Loss on drying (see Loss on Drying 731) is used in those cases where the loss sustained on heating may be not entirely water. 在加热时的持续失重可能不全是水分的情况下,使用标题干燥失重(见干燥失重<731>)。 METHOD I (TITRIMETRIC) 方法I(滴定测量法) Determine the water by Method Ia, unless otherwise specified in the individual monograph. 除非具体各论中另有规定,使用方法Ia来测定水分。 Method Ia (Direct Titration) 方法Ia(直接滴定) Principle— The titrimetric determination of water is based upon the quantitative reaction of water with an anhydrous solution of sulfur dioxide and iodine in the presence of a buffer that reacts with hydrogen ions. 原理:水分的滴定法检测是基于水与二氧化硫的无水溶液以及存在于缓冲液中与氢离子反应的碘之间的定量反应。 In the original titrimetric solution, known as Karl Fischer Reagent, the sulfur dioxide and iodine are dissolved in pyridine and methanol. The test specimen may be titrated with the Reagent directly, or the analysis may be carried out by a residual titration procedure. The stoichiometry of the reaction

美国药典USP气相色谱柱对照表

美国药典USP气相色谱柱对照表 L62 C30硅胶键合于完全多孔球状硅胶,粒径3~15μm。 G48 Highly polar, partially cross-linked cyanopolysiloxane. Rt-2560 G46 14% 氰丙基苯基- 86% 甲基聚硅氧烷 CB-1701MXT?-1701Rtx?-1701VF-1701ms OV-1701CBX-1701DB-1701DB-1701P G43 6% 氰丙基苯基- 94% 二甲基聚硅氧烷 MXT?-624DB-624MXT?-Volatiles CBX-1301 MXT?-1301OV-1301CB-624Rtx?-1301 VF-624ms/VF-1301ms Rtx?-624CB-1301CBX-624 G42 35% 苯基- 65% 二甲基乙烯聚硅氧烷 DB-35Rtx?-35MXT?-35CBX-35 HP-35DB-35MS G38 固定相G1 加减尾剂 MXT-1Rtx?-1MS Rtx?-1 G36 1% 乙烯基- 5% 苯基甲基聚硅氧烷 Rtx?-5MS Rtx?-5CBX-5MXT?-5 G35 聚乙二醇和硝基对苯二甲酸二乙二醇酯 DB-FFAP HP-FFAP CB-FFAP G32 20% Phenylmethyl-80% dimethylpolysiloxane. MXT?-20 G27 5% 苯基- 95% 甲基聚硅氧烷 CB-5XTI?-5Rtx?-5SIL MS VF-5ms Rtx?-5PONA HP-5MS HP-5DB-5MS SE-52DB-5SE-54 G25 聚乙二醇TPA(Carbowax 20M 对苯二酸) FFAP CBX-FFAP G19 25% 苯基- 25% 氰丙基甲基聚硅氧烷 OV-225Rtx?-225VF-23ms CBX-225 G17 75% 苯基- 25% 甲基聚硅氧烷 MXT?-65 G16 聚乙二醇(平均分子量15,000) DB-WAX CBX-Wax CB-WAX Stabilwax?PEG-20M Stabilwax?-DB Stabilwax?-DA MXT?-WAX

美国药典USP40-左氧氟沙星API

USP 40 Official Monographs / Levofloxacin 4831 Acceptance criteria: See Table 1. Sample solution: 1mg/mL of Levofloxacin in Mobile phase Chromatographic system Table 1(See Chromatography ?621?, System Suitability .)Relative Relative Acceptance Mode: LC Retention Response Criteria,Detector: UV 360 nm Name Time Factor NMT (%) Column: 4.6-mm × 25-cm; 5-μm packing L1Levodopa related Column temperature: 45°compound A 0.90.830.1Flow rate: 0.8mL/min Injection size: 25μL Levodopa 1.0——System suitability Levodopa related Sample: Standard solution compound B 2.8 0.83 0.5 Suitability requirements 5,6-Dihydroxy-in-Tailing factor: 0.5–1.5 dole-2-carboxylic Relative standard deviation: NMT 1.0%acid 6.0 2.5 0.1Analysis 0.1Samples: Standard solution and Sample solution individual Calculate the percentage of levofloxacin (C 18H 20FN 3O 4)— 0.3 total in the portion of Levofloxacin taken: Unknown impurities 1.0unknown Total impurities — — 1.1 Result = (r U /r S ) × (C S /C U ) × 100 r U = peak response of levofloxacin from the Sample ADDITIONAL REQUIREMENTS solution ?P ACKAGING AND S TORAGE : Preserve in tight, light-resistant r S = peak response of levofloxacin from the containers, in a dry place, and prevent exposure to ex-Standard solution cessive heat. C S = concentration of USP Levofloxacin RS in the ?USP R EFERENCE S TANDARDS ?11?Standard solution (mg/mL) USP Levodopa RS C U = concentration of Levofloxacin in the Sample USP Levodopa Related Compound A RS solution (mg/mL) 3-(3,4,6-Trihydroxyphenyl)alanine.Acceptance criteria: 98.0%–102.0% on the anhydrous C 9H 11NO 5213.19 basis USP Levodopa Related Compound B RS 3-Methoxytyrosine.IMPURITIES C 10H 13NO 4211.22 ?R ESIDUE ON I GNITION ?281?: NMT 0.2%. Use a platinum crucible. Delete the following: Levofloxacin ??H EAVY M ETALS , Method II ?231?: NMT 10ppm ?(Official 1-Jan-2018) ?O RGANIC I MPURITIES , P ROCEDURE 1 [N OTE —Procedure 1 is recommended if levofloxacin N -ox-ide is a potential organic impurity. Procedure 2 and Pro-cedure 3 are recommended if levofloxacin related com-pound B is a potential organic impurity.] Solution A, Mobile phase, Sample solution, and Chro-matographic system: Proceed as directed in the C 18H 20FN 3O 4·1/2H 2O 370.38Assay . 7H -Pyrido[1,2,3-de ]-1,4-benzoxazine-6-carboxylic acid, System suitability solution: 1mg/mL of USP Levoflox-9-fluoro-2,3-dihydro-3-methyl-10-(4-methyl-1-piperazinyl)-acin RS in Mobile phase 7-oxo-hydrate (2:1), (S )-; Sensitivity solution: 0.3μg/mL of USP Levofloxacin RS (?)-(S )-9-Fluoro-2,3-dihydro-3-methyl-10-(4-methyl-1-piper-in Mobile phase azinyl)-7-oxo-7H -pyrido[1,2,3-de ]-1,4-benzoxazine-6-car-System suitability boxylic acid, hemihydrate [138199-71-0].Samples: System suitability solution and Sensitivity Anhydrous [100986-85-41]. solution Suitability requirements DEFINITION Relative standard deviation: NMT 1.0%, System suit-Levofloxacin contains NLT 98.0% and NMT 102.0% of ability solution C 18H 20FN 3O 4, calculated on the anhydrous basis.Signal-to-noise ratio: NLT 10, Sensitivity solution IDENTIFICATION Analysis ?A . I NFRARED A BSORPTION ?197K ? Sample: Sample solution ?B . The retention time of the major peak of the Sample Calculate the percentage of each individual impurity in solution corresponds to that of the Standard solution , as the portion of Levofloxacin taken: obtained in the Assay.Result = (r U /r S ) × (1/F ) × 100 ASSAY ?P ROCEDURE r U = peak response of each impurity Buffer: 8.5g/L of ammonium acetate, 1.25g/L of cu-r S = peak response of levofloxacin pric sulfate, pentahydrate, and 1.3g/L of L -isoleucine in F = relative response factor (see Table 1)water Acceptance criteria: See Table 1. Mobile phase: Methanol and Buffer (3:7) Standard solution: 1mg/mL of USP Levofloxacin RS in Mobile phase USP Monographs

美国药典USP31(921)翻译版(下)

Method Ib (Residual Titration) 方法Ib(残留滴定)Principle— See the information given in the section Principle under Method Ia. In the residual titration, excess Reagent is added to the test specimen, sufficient time is allowed for the reaction to reach completion, and the unconsumed Reagent is titrated with a standard solution of water in a solvent such as methanol. The residual titration procedure is applicable generally and avoids the difficulties that may be encountered in the direct titration of substances from which the bound water is released slowly. 原理:见方法Ia项下原理部分给出的信息。在残留滴定中,额外的试剂被加入到供试样品中,为反应的完成留下了充分的时间,并且将未消耗掉的试剂与水和某种溶剂(例如,甲醇)的标准溶液一起滴定。残留滴定程序通常是可行的,并避免了可能在直接滴定该物质过程中遇到的困难,这些物质中被束缚水分释放得很缓慢。 Apparatus, Reagent, and Test Preparation— Use Method Ia. 仪器、试剂、供试配制液:同方法Ia。 Standardization of Water Solution for Residual Titration— Prepare a Water Solution by diluting 2 mL of water with methanol or other suitable solvent to 1000 mL. Standardize this solution by titrating 25.0 mL with the Reagent, previously standardized as directed under Standardization of the Reagent. Calculate the water content, in mg per mL, of the Water Solution taken by the formula: 用于残留滴定的水溶液的标准化:以甲醇或其他适当溶剂将2mL水稀释至1000mL,以配制水溶液。使用此前已经按照试剂的标准化项下规定进行过标准化的试剂,对25mL此溶液进行滴定,从而对其进行标准化。按照下面的公式,计算此水溶液中的水分含量(单位mg/mL): V F/25,

美国药典USP31翻译版

Many Pharmacopeial articles either are hydrates or contain water in adsorbed form. As a result, the determination of the water content is important in demonstrating compliance with the Pharmacopeial standards. Generally one of the methods given below is called for in the individual monograph, depending upon the nature of the article. In rare cases, a choice is allowed between two methods. When the article contains water of hydration, the Method I (Titrimetric), the Method II (Azeotropic), or the Method III (Gravimetric) is employed, as directed in the individual monograph, and the requirement is given under the heading Water.很多药典物品要么是水合物,要么含有处于吸附状态的水。因此,测定水分含量对于证实与药典标准的符合性是很重要的。通常,在具体的各论中会根据该物品的性质,要求使用下面若干方法中的一个。偶尔,会允许在2个方法中任选一个。当该物品含有水合状态的水,按照具体各论中的规定,使用方法I(滴定测量法)、方法II(恒沸测量法)、或方法III(重量分析法),这个要求在标题水分项下给出。 The heading Loss on drying (see Loss on Drying 731) is used in those cases where the loss sustained on heating may be not entirely water. 在加热时的持续失重可能不全是水分的情况下,使用标题干燥失重(见干燥失重<731>)。 METHOD I (TITRIMETRIC) 方法I(滴定测量法) Determine the water by Method Ia, unless otherwise specified in the individual monograph.除非具体各论中另有规定,使用方法Ia来测定水分。 Method Ia (Direct Titration) 方法Ia(直接滴定) Principle—The titrimetric determination of water is based upon the quantitative reaction of water with an anhydrous solution of sulfur dioxide and iodine in the presence of a buffer that reacts with hydrogen ions. 原理:水分的滴定法检测是基于水与二氧化硫的无水溶液以及存在于缓冲液中与氢离子反应的碘之间的定量反应。 In the original titrimetric solution, known as Karl Fischer Reagent, the sulfur dioxide and iodine are dissolved in pyridine and methanol. The test specimen may be titrated with the Reagent directly, or the analysis may be carried out by a residual titration procedure. The stoichiometry of the reaction is not exact, and the reproducibility of a determination depends upon such factors as the relative concentrations of the Reagent ingredients, the

USP美国药典,二甘醇、乙二醇及其他杂质

Glycerin C 3H 8O 3 92.10 1,2,3-Propanetriol. Glycerol [56-81-5]. ? Glycerin contains not less than 99.0 percent and not more than 101.0 percent of C 3H 8O 3, calculated on the anhydrous basis. The amount of any individual impurity, excluding diethylene glycol and ethylene glycol, if detected, meets the requirements under Other Impurities (NMT 0.1%) and the amount of total impurities, including diethylene glycol and ethylene glycol, is NMT 1.0%. Packaging and storage— Preserve in tight containers. USP Reference standards 11— USP Diethylene Glycol RS . USP Ethylene Glycol RS . USP Glycerin RS . Color— Its color, when viewed downward against a white surface in a 50-mL color-comparison tube, is not darker than the color of a standard made by diluting 0.40 mL of ferric chloride CS with water to 50 mL and similarly viewed in a color-comparison tube of approximately the same diameter and color as that containing the Glycerin. Identification— [NOTE—Compliance is determined by meeting the requirements for both Identification A and B .] A: Infrared Absorption 197F . B: Standard stock solution 1—Transfer 50 mg of USP Diethylene Glycol RS , accurately weighed, to a 100-mL volumetric flask, dilute with methanol to volume, and mix. Standard stock solution 2— Transfer 50 mg of USP Ethylene Glycol RS , accurately weighed, to a 100-mL volumetric flask, dilute with methanol to volume, and mix. Standard stock solution 3— Transfer 50 mg of USP Glycerin RS , accurately weighed, to a 100-mL volumetric flask, dilute with methanol to volume, and mix. Resolution solution— Transfer 5.0 mL each of Standard stock solution 1, Standard stock solution 2, and Standard stock solution 3, to a 100-mL volumetric flask, dilute with

美国药典USP32-重金属测试

<231>重金属本试验系在规定的试验条件下,金属离子与硫化物离子反应显色,通过制备的标准铅溶液目视比较测定,以确证供试品中重金属杂质含量不超过各论项下规定的限度(以供试品中铅的百分比表示,以重量计)。(见分光光度法和光散射项下测定法目视比较法<851>)[注意: 对本试验有响应的典型物质有铅、汞、铋、砷、锑、锡、镉、银、铜和钼等]。 除各论另有规定外,按第一法测定重金属。第一法适用于在规定试验条件下,能产生澄清、无色溶液的物质。第二法适用于在第一法规定试验条件下不能产生澄清、无色溶液的物质,或者适用于由于性质复杂,易干扰硫化物离子与金属离子形成沉淀的物质,或者是不易挥发的和易挥发的油类物质。第三法为湿消化法,仅用于第一法、第二法都不适合的情况。特殊试剂特殊试剂硝酸铅贮备液—取硝酸铅159.8mg,溶于100ml水中,加1ml硝酸,用水稀释至1000ml。制备和贮存本溶液的玻璃容器应不含可溶性铅。标准铅溶液—使用当天,取硝酸铅贮备液10.0ml,用水稀释至100.0ml。每1ml的标准铅溶液含相当于10μg的铅。按每克供试品取100μl标准铅溶液制备的对照溶液,相当于供试品含百万分之一的铅。方法方法II pH3.5醋酸盐缓冲液—取醋酸铵25.0g溶于25ml水中,加6N盐酸液38.0ml,必要时,用6N氢氧化铵液或6N盐酸液调节pH至3.5,用水稀释至100ml,混匀。标准溶液准备—精密量取标准铅溶液 2ml,(相当于20μg的Pb),置50ml比色管中,加水稀释至25ml,以精密pH 试纸作为外指示剂,用1N醋酸液或6N氢氧化铵液调节pH至3.0~4.0,用水稀释至40ml,混匀。供试品溶液制备—取各论项下规定的供试品溶液25ml,置50ml比色管中,或用各论项下规定用量的酸溶解样品,再用水稀释至25ml,供试品以g计,按下式计算:2.0/(1000L)式中L是重金属限度(%)。以精密pH试纸作为外指示剂,用1N醋酸液或6N氢氧化铵液调节pH至3.0~4.0,用水稀释至40ml,摇匀。对照溶液制备—取供试品溶液制备项下的溶液25ml,置50ml比色管中,加标准铅溶液2.0ml,以精密pH试纸作为外指示剂,用1N醋酸液或6N氢氧化铵液调节pH至3.0~4.0,用水稀释至40ml,摇匀。测定法—在上述三试管中,分别加入pH3.5的醋酸盐缓冲液2ml,然后再加硫代乙酰胺—甘油试液1.2ml,用水稀释至50ml,混匀,放置2分钟,在白色平面?自上向下观察:

USP《671》美国药典-包装容器——性能检测译文

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