USP美国药典 232 元素杂质-限度

First Supplement to USP 40–NF 35Chemical Tests / á232? Elemental Impurities—Limits 8065

á232? ELEMENTAL IMPURITIES—LIMITS

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INTRODUCTION

or drug products. These impurities may occur naturally, be added intentionally, or be introduced inadvertently (e.g., by inter-actions with processing equipment and the container–closure system). When elemental impurities are known to be present, have been added, or have the potential for introduction, assurance of compliance to the specified levels is required. A risk-based control strategy may be appropriate when analysts determine how to assure compliance with this standard. Due to the

SPECIATION

The determination of the oxidation state, organic complex, or combination is termed “speciation”. Each of the elemental impurities has the potential to be present in differing oxidation or complexation states. However, arsenic and mercury are of particular concern because of the differing toxicities of their inorganic and complexed organic forms.

The arsenic limits are based on the inorganic (most toxic) form. Arsenic can be measured using a total-arsenic procedure under the assumption that all arsenic contained in the material under test is in the inorganic form. Where the limit is exceeded using a total-arsenic procedure, it may be possible to show, via a procedure that quantifies the different forms, that the inor-ganic form meets the specification.

The mercury limits are based upon the inorganic (2+) oxidation state. The methyl mercury form (most toxic) is rarely an issue for pharmaceuticals. Thus, the limit was established assuming the most common (mercuric) inorganic form. Limits for articles that have the potential to contain methyl mercury (e.g., materials derived from fish) are to be provided in the monograph.Change to read:

ROUTES OF EXPOSURE

determined for each of the elemental impurities of interest for three routes of administration: oral, parenteral, and inhalational.These limits are based on chronic exposure. Consider the oral permissible daily exposures (PDEs) in Table 1 as a starting point in developing specific PDEs for other routes of administration, except where otherwise stated in the individual monograph.[N OTE —The routes of administration of drug products are defined in Pharmaceutical Dosage Forms á1151?

.]Change to read:

DRUG PRODUCTS

Table 1 are the base daily dose PDEs of the

Parenteral Products

Parenteral drug products with maximum daily volumes up to 2 L may use the maximum daily volume to calculate permissi-missible concentrations from PDEs.

8066 á232? Elemental Impurities—Limits / Chemical Tests

First Supplement to USP 40–NF 35

First Supplement to USP 40–NF 35Chemical Tests / á232? Elemental Impurities—Limits 8067

Recommendations for Elements to be Considered in the Risk Assessment

Table 2 identifies elemental impurities for inclusion in the risk assessment. This table can be applied to all sources of elemen-tal impurities in the drug product.

Options for Demonstrating Compliance

DRUG PRODUCT ANALYSIS OPTION

The results obtained from the analysis of a typical dosage unit, scaled to a maximum daily dose, are compared to the Daily Dose PDE.

Daily Dose PDE3 measured value (m g/g) × maximum daily dose (g/day)

The measured amount of each impurity is NMT the Daily Dose PDE, unless otherwise stated in the individual monograph.

SUMMATION OPTION

Separately, add the amounts of each elemental impurity (in m g/g) present in each of the components of the drug product:

Daily Dose PDE3 [S M

1(C

M

× W

M

)] × D

D

M= each ingredient used to manufacture a dosage unit

C M = element concentration in component (drug substance or excipient) (m g/g)

W

M = weight of component in a dosage unit (g/dosage unit)

D D = number of units in the maximum daily dose (unit/day)

The result of the summation of each impurity is NMT the Daily Dose PDE, unless otherwise stated in the individual mono-graph. Before products can be evaluated using this option, the manufacturer must ensure that additional elemental impurities cannot be inadvertently added through the manufacturing process or via the container–closure system over the shelf life of the product.

INDIVIDUAL COMPONENT OPTION

For drug products with a daily dose of NMT 10g, if all drug substances and excipients in a formulation meet the concentra-tion limits shown in Table 3, then these components may be used in any proportion. No further calculation is necessary. While elemental impurities derived from the manufacturing process or the container–closure system are not specifically provided for in the Individual Component Option, it is expected that the drug product manufacturer will ensure that these sources do not contribute significantly to the total content of elemental impurities.

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DRUG SUBSTANCE AND EXCIPIENTS

products dosed at a maximum daily dose of 10g/day. These values serve as default concentration limits to aid discussions be-tween drug product manufacturers and the suppliers of the components of their drug products. [N OTE—Individual compo-nents may need to be limited at levels different from those in the table depending on monograph-specific mitigating factors.]

8068á232? Elemental Impurities—Limits / Chemical Tests First Supplement to USP 40–NF 35

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ANALYTICAL TESTING

If, by process monitoring and supply-chain control, manufacturers can demonstrate compliance, then further testing may Elemental Impurities—Procedures á233?OTHER TESTS AND ASSAYS

Delete the following:

All radioactive determinations required by this method should be made with a suitable counting assembly over a period of time optimal for the particular counting assembly used. All procedures should be performed in replicate to obtain the greatest accuracy.

USP REFERENCE STANDARD á11?

USP Cyanocobalamin RS .

CYANOCOBALAMIN TRACER REAGENT

Dilute an accurately measured volume of a solution of radioactive cyanocobalamin* with water to yield a solution having a radioactivity between 500 and 5000 counts per minute per mL. Add 1 drop of cresol per L of solution prepared, and store in a refrigerator.

Standardization

Prepare a solution of a weighed quantity of USP Cyanocobalamin RS in water to contain 20 to 50 m g per mL. Perform the entire assay on a 10.0-mL portion of this solution, proceeding as directed under Assay Preparation , beginning with “Add water to make a measured volume.”

First Supplement to USP 40–NF 35

Chemical Tests / á371? Cobalamin Radiotracer Assay 8069

溶出度检查法美国药典USP-711

<711> DISSOLUTION 溶出度 (USP39-NF34 Page 540) General chapter Dissolution <711> is being harmonized with the corresponding texts of the European Pharmacopoeia and/or the Japanese Pharmacopoeia. These pharmacopeias have undertaken to not make any unilateral change to this harmonized chapter. 通则<711>溶出度与欧盟药典和日本药典中的相应部分相统一。这三部药典承诺不做单方面的修改。 Portions of the present general chapter text that are national USP text, and therefore not part of the harmonized text, are marked with symbols to specify this fact. 本章中的部分文字为本国USP内容，并没有与其他药典统一。此部分以（）标注。 This test is provided to determine compliance with the dissolution requirements where stated in the individual monograph for dosage forms administered orally. In this general chapter, a dosage unit is defined as 1 tablet or 1 capsule or the amount specified. Of the types of apparatus designs described herein, use the one specified in the individual monograph. Where the label states that an article is enteric coated and a dissolution or disintegration test does not specifically state that it is to be applied to delayed-release articles and is included in the individual monograph, the procedure and interpretation given for Delayed-Release Dosage Forms are applied, unless otherwise specified in the individual monograph. 本测试用于检测药品口服制剂的溶出度是否符合各论中的规定。本章中，除另有规定外，单位制剂定义为1片或1粒胶囊。对于本章中所述多种仪器，使用各论中规定的种类。除各论中另有规定外，如果检品是肠溶衣片且各论中的溶出度或崩解时限检查项下没有特别指出适用迟释剂的，使用本章中适用于迟释剂的流程和解释。 FOR DOSAGE FORMS CONTAINING OR COATED WITH GELATIN涂有或包含明胶的剂型 If the dosage form containing gelatin does not meet the criteria in the appropriate Acceptance Table (see Interpretation, Immediate-Release Dosage Forms, Extended-Release Dosage Forms, or Delayed-Release Dosage Forms) because of evidence of the presence of cross-linking, the dissolution procedure should be repeated with the addition of enzymes to the medium, as described below, and the dissolution results should be evaluated starting at the first stage of the appropriate Acceptance Table. It is not necessary to continue testing through the last stage (up to 24 units) when criteria are not met during the first stage testing, and evidence of cross-linking is observed. 如果剂型中含有明胶，其不符合验收表中的标准（见判断，速释制剂，延释制剂，缓释制剂），因为存在明胶交联结合作用，它的溶解过程与外加的媒介酶是重复的，见下面的描述，并且溶解结果可以通过适当的验收表的开始的第一阶段标准进行评估。如果溶出结果不满足第一阶段的测试标准，那么就没有必要继续测试到最后阶段，并且也证明了明胶交联结合作用的存在。

美国药典(USP)规定的色谱柱编号

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美国药典USP31 71 无菌检查法中文版

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USP《671》美国药典-包装容器——性能检测译文

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USP美国药典 233元素杂质-检查法

á233? ELEMENTAL IMPURITIES—PROCEDURES INTRODUCTION This chapter describes two analytical procedures (Procedures 1 and 2) for the evaluation of the levels of the elemental impuri-ties. The chapter also describes criteria for acceptable alternative procedures. By means of validation studies, analysts will confirm that the analytical procedures described herein are suitable for use on specified material. Use of Alternative Procedures The chapter also describes criteria for acceptable alternative procedures. Alternative procedures that meet the validation re-quirements herein may be used in accordance with General Notices and Requirements 6.30, Alternative and Harmonized Meth-ods and Procedures . Information on the Requirements for Alternate Procedure Validation is provided later in this chapter.Speciation The determination of the oxidation state, organic complex, or combination is termed speciation . Analytical procedures for spe-ciation are not included in this chapter, but examples may be found elsewhere in USP–NF and in the literature. PROCEDURES ? C OMPENDIAL P ROCEDURES 1 AND 2 System standardization and suitability evaluation using applicable reference materials should be performed on the day of analysis. Procedure and detection technique:Procedure 1 can be used for elemental impurities generally amenable to detection by inductively coupled plasma–atomic (optical) emission spectroscopy (ICP–AES or ICP–OES). Procedure 2 can be used for ele-mental impurities generally amenable to detection by ICP–MS. Before initial use, the analyst should verify that the proce- dure is appropriate for the instrument and sample used (procedural verification) by meeting the alternative procedure vali-dation requirements below. Sample preparation:Forms of sample preparation include Neat , Direct aqueous solution , Direct organic solution , and Indi- rect solution . The selection of the appropriate sample preparation depends on the material under test and is the responsibil-ity of the analyst. When a sample preparation is not indicated in the monograph, an analyst may use any of the following appropriately validated preparation procedures. In cases where spiking of a material under test is necessary to provide an acceptable signal intensity, the blank should be spiked with the same Target elements , and where possible, using the same spiking solution. Standard solutions may contain multiple Target elements . [N OTE —All liquid samples should be weighed.]Neat:Used for liquids or alternative procedures that allow the examination of unsolvated samples. Direct aqueous solution:Used when the sample is soluble in an aqueous solvent. Direct organic solution:Used where the sample is soluble in an organic solvent. Indirect solution:Used when a material is not directly soluble in aqueous or organic solvents. Total metal extraction is the preferred sample preparation approach to obtain an Indirect solution . Digest the sample using the Closed vessel diges-tion procedure provided below or one similar to it. The sample preparation scheme should yield sufficient sample to allow quantification of each element at the limit specified in the corresponding monograph or chapter. Closed vessel digestion:This sample preparation procedure is designed for samples that must be digested in a Concen-trated acid using a closed vessel digestion apparatus. Closed vessel digestion minimizes the loss of volatile impurities. The choice of a Concentrated acid depends on the sample matrix. The use of any of the Concentrated acids may be appropri-ate, but each introduces inherent safety risks. Therefore, appropriate safety precautions should be used at all times. [N OTE —Weights and volumes provided may be adjusted to meet the requirements of the digestion apparatus used.] An example procedure that has been shown to have broad applicability is the following. Dehydrate and predigest 0.5 g of primary sample in 5 mL of freshly prepared Concentrated acid . Allow to sit loosely covered for 30 min in a fume hood.Add an additional 10 mL of Concentrated acid , and digest, using a closed vessel technique, until digestion or extraction is complete. Repeat, if necessary, by adding an additional 5 mL of Concentrated acid . [N OTE —Where closed vessel digestion is necessary, follow the manufacturer’s recommended procedures to ensure safe use.] Alternatively, leachate extraction may be appropriate with justification following scientifically validated metal disposition studies, which may include animal studies, speciation, or other means of studying disposition of the specific metal in the drug product. Reagents:All reagents used for the preparation of sample and standard solutions should be free of elemental impurities,in accordance with Plasma Spectrochemistry á730?. ? P ROCEDURE 1: ICP–OES Standardization solution 1: 1.5J of the Target element(s) in a Matched matrix Standardization solution 2:0.5J of the Target element(s) in a Matched matrix Sample stock solution:Proceed as directed in Sample preparation above. Allow the sample to cool, if necessary. For mer-cury determination, add an appropriate stabilizer. Sample solution:Dilute the Sample stock solution with an appropriate solvent to obtain a final concentration of the Target elements at NMT 1.5J . Blank: Matched matrix 298 á233? Elemental Impurities—Procedures / Chemical Tests USP 40

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

USP色谱柱解释

L1和L8是美国药典(USP)规定的色谱柱编号，其实就是C18柱和NH2柱。下面是对应的色谱柱类型。 L1：十八烷基键合多孔硅胶或无机氧化物微粒固定相，简称C18或ODS L2：30～50um表面多孔薄壳型键合C18(ODS)固定相 L3：多孔硅胶微粒即一般的硅胶柱 L4：30～50um表面多孔薄壳型硅胶 L5：30～50um表面多孔薄壳型氧化铝 L6：30～50um实心微球表面包覆磺化碳氟聚合物－强阳离子交换固定相 L7：全多孔硅胶微粒键合C8官能团固定相简称C8柱 L8：全多孔硅胶微粒键合非交联NH2固定相简称NH2柱 L9：强酸性阳离子交换基团键合全多孔不规则形硅胶固定相 L10：多孔硅胶微球键合氰基固定相（CN）简称CN柱 L11：键合苯基多孔硅胶微球固定相简称苯基柱 L12：无孔微球键合季胺功能团的强阴离子填料 L13：三乙基硅烷化学键合全多孔硅胶微球固定相（C1）简称C1柱 L14:10um硅胶化学键合强碱性季铵盐阴离子交换固定相简称SAX柱 L15：已基硅烷化学键合全多孔硅胶微球固定相简称C6柱 L16：二甲基硅烷化学键合全多孔硅胶微粒固定相 L17：氢型磺化交联苯乙烯-二乙烯基苯共聚物,强阳离子交换树脂 L18: 3～10um全多孔硅胶化学键合胺基（NH2）和氰基（CN） L19：钙型磺化交联苯乙烯－二乙烯基苯共聚物，强阳离子交换树脂 L20：二羟基丙烷基化学键合多孔硅胶微球固定相（Diol）简称二醇基柱 L21：刚性苯乙烯－二乙烯基苯共聚物微球 L22：带有磺酸基团的多孔苯乙烯阳离子交换树脂 L23：带有季胺基团的聚甲基丙烯酸甲酯或聚丙烯酸酯多孔离子交换树脂 L24：表面含有大量羟基的半刚性聚乙烯醇亲水凝胶 L25：聚甲基丙烯酸酯树脂交联羟基醚（表面含有残余羧基功能团）树脂。能分离分子量100～5000MW范围的水溶性中性、阳离子型及阴离子型聚合物（用聚氧乙烯测定）的固定相 L26：丁基硅烷化学键合全多孔硅胶微球固定相 L27：30～50um的全多孔硅胶微粒

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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