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1997 년 7 월 8 일 CPMP/CVMP/QWP/115/95 COMMITTEE FOR PROPRIETARY MEDICINAL PRODUCTS (CPMP) COMMITTEE FOR VETERINARY MEDICINAL PRODUCTS (CVMP) 항산화제와항미생물보존제의의약품포함에관한가이드라인 (NOTE FOR GUIDANCE ON INCLUSION OF ANTIOXIDANTS AND ANTIMICROBIAL PRESERVATIVES IN MEDICINAL PRODUCTS) 5-6 October 1995 Discussion in the Quality Working Party (QWP) 1-2 February 1996 4-5 July 1996 Discussion in the Biotechnology Working Party (BWP) 10-11 June 1996 Transmission to the CPMP and CVMP July 1996 Transmission to Interested Parties July 1996 Deadline for Comments 31 January 1997 Discussion in the Quality Working Party (QWP) 4-5 June 1997 Final Approval by CPMP and CVMP July 1997 Date for Coming into Operation (Studies Commencing After) January 1998 www..co.kr 1

INCLUSION OF ANTIOXIDANTS AND ANTIMICROBIAL PRESERVATIVES IN MEDICINAL PRODUCTS 1. 서론 (INTRODUCTION) Antioxidants and Antimicrobial Preservatives are substances which are used to extend the shelf-life of medicines by respectively retarding the oxidation of active ingredients and excipients, and by reducing microbial proliferation. 항산화제와항미생물보존제는각기활성성분과첨가물의산화를저해하고미생물증식을억제하여의약품의유효기간을연장시키는데사용되는성분이다. The properties of these substances are due to certain chemical groups which are usually aggressive towards living cells and which lead to certain risks when used in man (and animals). 이들성분의특징은일반적으로살아있는세포를공격하는특정화학기에의한것이며, 사람 ( 과동물 ) 에사용하면위해를유발하기도한다. The purpose of this note for guidance is to describe the information that needs to appear in applications for marketing authorisations with regard to the addition of any antioxidants or antimicrobial preservatives. For each antioxidant and antimicrobial preservative the application should contain: 이문서의목적은항산화제나항미생물보존제의투입과관련하여판매허가신청서류에포함시킬필요가있는정보를제시하는데있다. 항산화제와항미생물보존제각각에대하여다음정보를신청서류에포함시켜야한다. reason for inclusion 투입이유 proof of efficacy 유효성증거 the method of control in the finished product 최종제품에서의관리방법 details of the labelling of the finished product 최종제품의표시사항 safety information www..co.kr 2

안전성정보 2. 항산화제 (ANTIOXIDANTS) Antioxidants are used to reduce the oxidation of active substances and excipients in the finished product. Antioxidants should not be used to disguise poorly formulated products or inadequate packaging. The need to include an antioxidant should be explained and fully justified. Oxidative degradation can be accelerated by light and by the presence of mineral impurities, due to the formation of free radicals. 항산화제는활성성분과첨가제의산화를감소시키는데사용된다. 부적절한포장이나부실하게조제된제품을은폐하기위한목적으로항산화제를사용해서는안된다. 항산화제의투입필요성을설명하고그타당성을충분히제시해야한다. 미네랄불순물이있고빛에노출되면, 자유라디칼의형성으로인하여산화반응이촉진될수있다. There are three types of antioxidants: 3 종류의항산화제가있다. Type Definition Example True antioxidants These are thought to block chain reactions by reacting with free radicals 자유라디칼과반응하여연쇄반응을차단하는것으로생각된다. Reducing agents These have a lower redox potential than the drug or excipient they are protecting 이항산화제의산화환원전위는보호대상첨가제나약물보다더낮다. Antioxidant These enhance the effects of synergists antioxidants 항산화제의효과를증진시킨다. butylated hydroxytoluene ascorbic acid sodium edetate The efficacy obtained for an antioxidant depends on its nature, its concentration, the stage at which it is incorporated into the finished product, the nature of the container and the formulation. 항산화제로인해획득되는유효성은항산화제의특성, 농도, 최종제품에투입되는단계, 용기의특성, 조성에따라달라진다. www..co.kr 3

The efficacy of antioxidants must be assessed in the finished product in conditions which simulate actual use by measuring the extent of degradation in the finished product, with and without the antioxidant. 최종제품의실제사용상황을시뮬레이션한조건에서분해정도 ( 항산화제가있는상태와없는상태 ) 를측정함으로써, 항산화제의유효성을평가해야한다. Antioxidants should only be included in a formulation if it has been proved that their use cannot be avoided. This applies to cases where the manufacturing process is optimised to minimise the potential for oxidation. 항산화제의사용을피할수없다는것이증명된경우에만항산화제를제제에포함시킨다. 산화가능성을최소화할수있게제조공정을최적화한경우에이를적용한다. 3. 항미생물보존제 (ANTIMICROBIAL PRESERVATIVES) Antimicrobial Preservatives are used to prevent or inhibit the growth of microorganisms which could present a risk of infection or degradation of the medicinal product. These microorganism may proliferate during normal storage conditions or use of the product by the patient, particularly in multidose preparations. 항미생물보존제는의약품의분해나감염위험을유발할수있는미생물의증식을예방또는저해하기위해사용한다. 이런미생물이정상적인보관조건이나환자의제품사용과정에서번식할수있다. 다용량제제인경우에특히그렇다. On no account should preservatives be used as an alternative to good manufacturing practice. 어떤경우에도보존제를 GMP 의대체방안으로활용해서는안된다. Preparations at greatest risk of contamination are those which contain water such as solutions, suspensions and emulsions to be taken orally, solution for external use, creams, and sterile preparations used repeatedly (e.g. injectable multidose preparations and eye-drops). 내용액제, 현탁제, 유제와외용액제, 크림제, 그리고반복적으로사용되는무균제제 ( 예, 다용량주사제, 안약 ) 과같이물을함유한제품이오염위험성이가장큰제제이다. The level of efficacy obtained will vary according to the chemical structure of the www..co.kr 4

preservative, its concentration, the physical and chemical characteristics of the medicinal product (especially ph) and the type and level of initial microbial contamination. The design of the pack and the temperature at which the product is stored will also affect the level of activity of any antimicrobial preservatives present. 유효성수준은보존제의화학적구조, 그의농도, 의약품의물리적 / 화학적특성 ( 특히 ph), 그리고최초미생물오염수준과그유형에따라다르다. 제품보관온도와포장디자인도항미생물보존제의활성에영향을준다. The antimicrobial efficacy of the preservative in the finished product should be assessed during product development using the European Pharmacopoeia test. 최종제품에함유된보존제의항미생물유효성을유럽약전방법에따라제품개발단계에서평가해야한다. If products do not contain a preservative and do not have adequate inherent preservative efficacy they must not be packaged in multidose presentations without a sound justification. 보존제를함유하고있지않으며적절한내재적보존제효과를갖지않는제품은, 타당한이유없이다용량포장을해서는안된다. 4. 조성 (FORMULATION) Antimicrobial preservative and antioxidants should be chemically defined (reference to existing pharmacopoeia monographs may be used) and designated by the Chemical Abstract Service (CAS) registry number if they are not referenced in the pharmacopoeia. 항미생물보존제와항산화제는화학적으로정의되어야하며 ( 기존약전모노그래프의참조가능 ), 약전에수재되지않은경우에는 CAS 번호를제시해야한다. The purpose for the inclusion of any antioxidant or antimicrobial preservative should be stated (antioxidant for the benefit of active ingredient or excipient or both, or antimicrobial preservative). 항산화제나항미생물보존제의포함목적을명시한다 ( 활성성분이나첨가제 ( 또는이둘모두 ) 를위한항산화제또는항미생물보존제 ). www..co.kr 5

5. 의약품개발경위 (DEVELOPMENT PHARMACEUTICS) During the pharmaceutical development of the product the applicant should demonstrate: 의약품개발단계에서신청업체는다음을증명해야한다. the necessity to add an antioxidant or a preservative to the finished product at the level chosen. 설정수준의항산화제또는보존제를최종제품에투입할필요성 the physical and chemical compatibility of the antioxidant and of the preservative with other constituents of the finished product, the container and the closures. 항산화제와보존제와최종제품의기타성분, 용기, 마개와의물리적 / 화학적조화성 The concentration used must be justified in terms of efficacy and safety, such that the minimum concentration of preservative is used which gives the required level of efficacy. The appropriate test method for efficacy of antimicrobial preservation is that of the European Pharmacopoeia. This should be used to determine whether the required level of activity is achieved. 사용농도의타당성을유효성과안전성측면에서제시해야한다. 필요수준의유효성을제공하는최소농도의보존제를사용한다. 항미생물보존유효성을평가하는시험방법은유럽약전에수재된것으로한다. 이방법을사용하여필요수준의활성이달성되는지결정한다. In the case of antioxidants, these should only be used once it has been shown that their use cannot be avoided, even if the manufacturing process is optimised to minimise the potential for oxidation, for example by manufacturing and filling products under an inert headspace gas. 예를들어불활성헤드스페이스가스아래에서제품을제조하고충전하는식으로산화가능성을최소화하는방향으로제조공정을최적화한경우라도, 항산화제의사용을피할수없다는것이증명된경우에만항산화제를사용해야한다. The safety of the antioxidant or preservative should be supported by bibliographic and / or experimental data. www..co.kr 6

항산화제나보존제의안전성을참고자료및 / 또는실험데이터를통해뒷받침해야한다. Some antioxidants or antimicrobial preservatives may be undesirable under certain circumstances e.g. mercury containing preservatives, benzyl alcohol (when used in parenteral products for children under the age of 2 years or in newborn animals or in cats), benzoic acid esters (when used in any medicinal products for injection), sulphites and metabisulphite. 특정상황에서는일부항산화제나항미생물보존제가바람직하지않을수있다 ( 예, 수은함유보존제, 벤질알코올 (2세이하어린이나갓태어난동물또는고양이에투여할비경구제품에사용할때 ), 벤조산에스테르 ( 주사제에사용할때 ), 아황산염, 중아황산염 ). Parenteral infusions do not contain any added antimicrobial preservatives and no antimicrobial preservatives are added when the medicinal product is intended for administration by routes where for medical reasons an antimicrobial preservative is unacceptable, such as intercisternally or by any other route of administration which gives access to the cerebrospinal fluid or retro-ocularly. 수액제는항미생물보존제를함유하지않으며, 의학적이유에서항미생물보존제를사용할수없는경로로투여하는경우에는 ( 예, 수조간주입또는뇌척수액이나안구후방에주입하는기타투여경로 ) 항미생물보존제를절대포함시키지않는다. 6. 첨가제의관리 (CONTROL OF THE EXCIPIENTS) Antimicrobial preservatives and antioxidants are defined as excipients and as such should be controlled following the guidance given in The Rules Governing Medicinal Products in the European Union, Volume III Excipients in the Dossier for Application for Marketing Authorisation of a Medicinal Product. 항미생물보존제와항산화제는첨가제에해당되며, 그러므로 EU 의약품관리규칙볼륨 III " 의약품판매허가신청서류중첨가제 " 에제시된가이드라인에따라관리해야한다. 7. 최종제품의관리 (CONTROL OF THE FINISHED PRODUCT) The finished product release specifications should include an identification test and limits for any antioxidants and antimicrobial preservatives present in the formulation. The finished product specification against which the product is tested throughout its shelf-life should also include limits for the antimicrobial preservatives www..co.kr 7

present. 최종제품출하승인규격에제제중의항산화제와항미생물확인시험과한도기준을포함시켜야한다. 또한유효기간전체에걸쳐제품시험의기준이되는최종제품규격에도항미생물보존제의한도기준을포함시켜야한다. Where antioxidants are used up during the manufacture of the product, the release limits should be justified by batch data. The adequacy of specified limits should be justified on the basis of controlled conditions and in-use stability testing to ensure that sufficient antioxidant remains to protect the product throughout its entire shelf-life and during the proposed in-use period. 제품제조시에항산화제를사용한다면, 배치데이터에의거하여출하승인한도기준의타당성을제시해야한다. 전체유효기간과예정사용기간동안제품보호에충분한항산화제가존재하도록하기위하여, 관리조건과사용시의안정성실험결과에근거해지정기준의적절성을타당하게증명한다. The control of antioxidants and antimicrobial preservatives should comply with the requirements identified in the guideline Specifications and control testing of the finished product. 항산화제와항미생물보존제의관리방법은 " 최종제품의규격과시험 " 에제시된기준에부합해야한다. 8. 안정성 (STABILITY) The application should follow the current CPMP and CVMP guidelines on the stability of new dosage forms and should ensure that antimicrobial preservative and antioxidants levels are quantified periodically throughout the shelf-life of the finished product. In addition the efficacy of preservatives should be established using the test for efficacy of antimicrobial preservation of the European Pharmacopoeia. This should be performed on the finished product at the end of the shelf-life and at the lower preservative limit in the end of shelf-life specification. The former is necessary, even if no evidence of degradation of the antimicrobial preservative and of the antioxidant is observed on storage, as other chemical and physical changes in the finished product may influence the efficacy of the antimicrobial preservative and of the antioxidant. 신규제형의안정성에관한현행 CPMP와 CVMP 가이드라인에따라안정성실험을 www..co.kr 8

실시해야하며, 항미생물보존제와항산화제의양을최종제품의유효기간전체에걸쳐주기적으로측정해야한다. 또한유럽약전의항미생물보존제유효성시험방법에의거하여보존제의유효성을확립한다. 유효기간말기의최종제품과유효기간규격의보존제하한한도기준상태인최종제품을상대로이평가를실시한다. 특히최종제품의다른화학적 / 물리적변화가항미생물보존제와항산화제의유효성에영향을줄수있으므로, 제품보관중의항미생물보존제와항산화제분해증거가관찰되지않더라도, 유효기간말기의최종제품평가가필요하다. In the case of products presented in multidose containers, the efficacy of the antimicrobial preservative under simulated in-use conditions must be established. The tests should be performed under the same condition as it is expected to be used by the user. It may also be appropriate to examine the efficacy of the antimicrobial preservative following storage of opened or used containers for the proposed in use shelf-life. 다회용량용기에포장된제품인경우, 시뮬레이션사용조건에서의항미생물보존제유효성을평가하여확립해야한다. 사용자의예상사용조건과동일한조건에서평가를실시한다. 또한개봉용기나사용용기를예정사용기간동안보관하고나서항미생물보존제의유효성을조사하는것도적절할수있다. Further details of in use testing for veterinary products is provided in the current CVMP Notes for Guidance on in use stability testing. 동물의약품의사용중시험에관한자세한사항은사용중의안정성실험에관한 CVMP 가이드라인을참조한다. 9. 표시사항 (LABELLING) Labelling must be in accordance with relevant Community Directives - Council Directive 92/27/EEC and 81/851/EEC. 표시사항은해당디렉티브 ( 이사회디렉티브 92/27/EEC 와 81/851/EEC) 를준수해야한다. However, if a product is presented in a multidose container without a preservative because: 하지만다음과같은이유로보존제없이다회용량용기에포장된제품인경우, www..co.kr 9

a) it is intended for single use only (e.g. cytotoxic), 일회용으로만사용될예정인경우 ( 예, 세포독성 ). b) the product is self-preserving, 제품자체가보존효과를갖는경우. c) the product is oils based, 제품이오일성인경우. the labelling and product literature should indicate the absence of a preservative. This would not only emphasise the increased risk associated with the use of such products, but also aid the physician to specifically identify a product without preservative. 표시자재와제품관련문서에보존제가없음을표시해야한다. 이때제품사용과관련한리스크의증가를강조하고, 보존제가없는제품을의사가구체적으로파악하는데도움이되도록한다. www..co.kr 10