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2009－2011年FDA警告信涉及HPLC的內(nèi)容 已有1人參與
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2009－2011年FDA警告信涉及HPLC的內(nèi)容 2012-03-10 11:54:53| 分類： 2009－2011年FDA警告信涉及HPLC的內(nèi)容 歐盟符合性研究院（ECA）Günter Brendelberger博士昨天（2012年2月28日）發(fā)布了：2009－2011年FDA警告信中涉及高效液相色譜法的主要問題。 在使用高效液相色譜（HPLC）存在的關(guān)鍵問題包括以下4個(gè)方面： 1.電子記錄的原始數(shù)據(jù)/保護(hù) 2.校準(zhǔn)/確認(rèn) 3.方法驗(yàn)證 4.系統(tǒng)的適用性/序列 原文鏈接： Go here to access the complete list of FDA findings regarding HPLC. 全部譯文如下： 2009–2011年FDA警告信涉及HPLC的內(nèi)容 1. Raw Data / Protection of Electronic Records 電子記錄的原始數(shù)據(jù)/保護(hù) Your firm lacks systems to ensure that all electronic data generated in your Quality Control laboratory is secure and remains unaltered. All analysts have system administrator privileges that allow them to modify, overwrite, and delete original raw data files … in the High Performance Liquid Chromatography (HPLC) units.貴公司缺乏系統(tǒng)以確保所有的在質(zhì)量控制實(shí)驗(yàn)室產(chǎn)生的電子數(shù)據(jù)是安全的并保持不變。你們HPLC崗位所有的分析員都具有系統(tǒng)管理員的權(quán)限去修改，覆蓋并刪除原始數(shù)據(jù)。 There are no procedures that address the security measures in place for generation and modification of electronic data files for these instruments used for raw material, in-process,finished product and stability testing. In addition, your firm's review of laboratory data does not include a review of an audit trail or revision history to determine if unapproved changes have been made. 沒有建立一個(gè)程序規(guī)定如何對(duì)原材料、中間控制、成品和穩(wěn)定性測(cè)試的電子文件進(jìn)行安全保存和修改。貴公司的實(shí)驗(yàn)室數(shù)據(jù)審查并不包括審計(jì)跟蹤或未經(jīng)批準(zhǔn)修改數(shù)據(jù)的歷史記錄審查。 For example,your firm has failed to periodically conduct back-up procedures This server was used to store, back-up, and/or archive raw test data from computer systems (Software:…controlling and monitoring… High-performance liquid chromatography (HPLC) systems in accordance to SOP …”.例如貴公司未能按SOP的要求對(duì)服務(wù)器上存貯的原始數(shù)據(jù)進(jìn)行定期備份。 Your response, however, is inadequate because you fail to adequately address whether you were able to recover the critical data not backed-up between August 2010 and when you first implemented the daily backup process. Your firm has yet to indicate whether HPLC raw data records could be retrieved for the duration of time that the … server was not backing-up the HPLC system data.你們的回復(fù)是不適當(dāng)?shù)�，因�(yàn)槟銈儾荒艹浞謹(jǐn)⑹?010年8月是否對(duì)關(guān)鍵數(shù)據(jù)進(jìn)行了備份，2010年8月是你們第一次執(zhí)行備份程序。貴公司還不能表明能否找到那段時(shí)間的HPLC原始數(shù)據(jù)，…服務(wù)器不支持備份HPLC系統(tǒng)數(shù)據(jù)。 Your firm's laboratory analysts have the ability to access and delete raw chromatographic data located on the … of … used to conduct HPLC testing. Due to this unrestrictive access, there is no assurance that laboratory records and raw data are accurate and valid.貴公司實(shí)驗(yàn)室分析員個(gè)具有訪問和刪除原始色譜數(shù)據(jù)的權(quán)力，你們這種不受限制的訪問無法保證實(shí)驗(yàn)記錄和原始數(shù)據(jù)的準(zhǔn)確性和有效性。 2. Calibration / Qualification 校準(zhǔn)/確認(rèn) You replaced the … HPLC systems operating on … software with … new qualified HPLC units from … software. This validation information will be reviewed at the next inspection. In addition, your response is inadequate because it lacks a retrospective evaluation of the data from the former HPLC units.你們回復(fù)說更換了高效液相色譜系統(tǒng)的操作軟件......我們將會(huì)在下次檢查中確認(rèn)你們進(jìn)行的驗(yàn)證相關(guān)文件。此外，你們的回復(fù)是不充足的，因?yàn)槿狈?duì)過去PHLC崗位數(shù)據(jù)的回顧性評(píng)價(jià)。 For the testing of incoming components, your firm failed to conduct HPLC system qualification using certified standards and validated procedures … . Your laboratory failed to certify … against a primary standard from an ccredited institution and/or to fully characterize the material as a standard.對(duì)進(jìn)廠組份檢驗(yàn)，貴公司不能使用權(quán)威部門的標(biāo)準(zhǔn)品對(duì)HPLC系統(tǒng)進(jìn)行確認(rèn)與驗(yàn)證。你們實(shí)驗(yàn)室未能證明你們使用的標(biāo)準(zhǔn)品是合法性，或從認(rèn)可機(jī)構(gòu)購置和/或從用基準(zhǔn)標(biāo)準(zhǔn)品標(biāo)定工作標(biāo)準(zhǔn)品。 Your firm failed to conduct injector and detector performance testing for the … HPLC system. For example, no HPLC injector and detector testing for linearity, accuracy, and precision were conducted, such as: 1) various injection volumes and standard concentration testing; 2) evaluation of detector for noise/drift; and 3) carryover testing to evaluate response at low levels to determine the detection of possible interferences that may affect peaks of interest.貴公司沒有對(duì)HPLC的注樣器和檢測(cè)器進(jìn)行性能測(cè)試。例如，沒有對(duì)HPLC注樣器和檢測(cè)器進(jìn)行線性，準(zhǔn)確度，精度度確認(rèn)。例如：1）不同注射量和標(biāo)準(zhǔn)液的測(cè)試；2）對(duì)檢測(cè)器的噪音/漂移評(píng)估；3）殘留試驗(yàn)，來評(píng)估低峰響應(yīng)時(shí)，確定可檢測(cè)出可能干擾主峰的殘留。 Your HPLC calibration lacks a carry over test (sample injection residual test), sample energy (intensity of light source), and lamp use hours determination.你們的HPLC校準(zhǔn)缺少進(jìn)樣殘留試驗(yàn)，能源（光源強(qiáng)度），燈泡使用時(shí)間的測(cè)定內(nèi)容。 Your firm also fails to maintain raw data associated with the re-qualification and calibration of your laboratory instruments. During the inspection the investigators were informed that the annual re-qualification and calibration of your laboratory equipment (e.g., HPLC, GC, polarimeter, and analytical balance) is performed by the … . However, you were unable to provide raw data or documentation regarding the qualification and calibration of your instruments and data to demonstrate that your quality unit reviewed and approved the work performed by your contractor. 貴公司不能對(duì)實(shí)驗(yàn)室儀器進(jìn)行重新確認(rèn)和校準(zhǔn)來維護(hù)原始數(shù)據(jù)。在考察期間調(diào)查員要求你們要對(duì)實(shí)驗(yàn)室設(shè)備進(jìn)行年度重新確認(rèn)和校準(zhǔn)（例如，高效液相色譜儀，氣相色譜，旋光儀，分析天平），然而你們無法提供重新確認(rèn)和校準(zhǔn)的原始數(shù)據(jù)或文件和質(zhì)量部門審核文件，和承包商審查的批準(zhǔn)文件。 3. Method Validation 方法驗(yàn)證 Your firm failed to generate and document chromatographic data to support the validation of the analytical method .. used for the determination of Urea in Urea Cream 40%. In addition, your firm failed to generate a and document chromatographic data to support stress studies …to demonstrate that the method is suitable for determining stability.貴公司沒有色譜數(shù)據(jù)來支持分析方法的驗(yàn)證......該方法用于40％尿素霜的測(cè)定。此外，貴公司沒有色譜數(shù)據(jù)來支持降解實(shí)驗(yàn)研究和該方法是否適用于穩(wěn)定性研究。 Your firm has not verified that the preservatives and API test methods using the … System is adequate for its intended use. The … system is different from the previously used … HPLC system in make, model, and column. In addition, your analysis of … in finished product does not identify the maximum adjustment in mobile phase to obtain a suitable resolution between peaks … .貴公司沒有確認(rèn)因使用不同HPLC儀器、型號(hào)、柱子時(shí)測(cè)定防腐劑和API方法是否適當(dāng)。此外，對(duì)某制劑的分析方法沒有確認(rèn)流動(dòng)相的最大調(diào)整量從而獲得合適的分離度。 You failed to include testing for method precision and ruggedness in your HPLC Assay Method Validation … . We are concerned that you have not established the degree of reproducibility or repeatability of the analytical procedure under normal operating conditions. In addition, you failed to establish adequate system suitability parameters to ensure that the complete testing system (including instrument, reagents, columns, and analysts) continues to operate suitably for the intended application.在HPLC分析方法驗(yàn)證中，你們沒有包括精度度和耐用性驗(yàn)證....我們關(guān)注的是你們不能建立在正常條件下重復(fù)性或重復(fù)性限度要求。此外，你們還沒有建立足夠的系統(tǒng)適用性參數(shù)來確保該測(cè)試系統(tǒng)（包括儀器，試劑，柱和分析師）符合預(yù)期的用途。 Your firm failed to include the following characteristics: accuracy, robustness, ruggedness and specificity in your validation of the HPLC assay method … used for the analysis of Pyridoxine Hydrochloride (Vitamin B6), Riboflavin 5' Phosphate Sodium (Vitamin B2) and Thiamine Hydrochloride (Vitamin B1) in Poly-Vitamin Drop products.在你們的HPLC分析方法驗(yàn)證中缺少準(zhǔn)確度，耐用性，再現(xiàn)性和專屬性的驗(yàn)證，該方法用于測(cè)定在聚維滴劑產(chǎn)品中維生素B6、核黃素維生素B2、維生素B1的測(cè)定。 4. System Suitability / Sequences系統(tǒng)的適用性/序列 Your GC and HPLC analyses for both finished products and raw materials lack appropriate system suitability determinations. Your SOP … each specify three standard solution injections. Both methods are used for testing of drug products at batch release and during stability study.你們的GC和HPLC在成品和原料的測(cè)定中缺乏適當(dāng)?shù)南到y(tǒng)適用性實(shí)驗(yàn)，這兩種方法都用于藥品的放行檢測(cè)和穩(wěn)定性研究。 Our concern is that you may not be evaluating the signal to noise ratio during system suitability. Evaluation of the signal to noise ratio during system suitability is a normal laboratory practice when testing low level impurities or degradant content by HPLC.我們關(guān)注的是你們可能未在系統(tǒng)適應(yīng)性中評(píng)估信噪比。當(dāng)用HPLC 檢測(cè)低含量的雜質(zhì)和降解產(chǎn)物時(shí)，通常在系統(tǒng)適應(yīng)性中評(píng)估信噪比。 Failure to ensure that approved test procedures for …. HPLC are followed. For example, the inspection found no scientific justification for the current sequence of chromatographic injections performed, which is different to the sequence included in the approved analytical method.沒有遵守已批準(zhǔn)的HPLC程序要求進(jìn)行檢測(cè)，例如在檢查中發(fā)現(xiàn)操作者使用沒有任何科學(xué)道理的色譜進(jìn)樣序列，也跟批準(zhǔn)的分析序列不同。 We remain concerned about current laboratory practices, in that not all injection results are being reported. For example, the assay test for lots … failed to include all the injection results performed as part of the chromatographic run. Your response provides no explanation regarding why analytical results are selectively reported. 我們?nèi)匀魂P(guān)注目前你們實(shí)驗(yàn)室還存在沒有被發(fā)現(xiàn)的其它做法。例如很多含量測(cè)試沒有包括實(shí)際運(yùn)行進(jìn)樣的所有色譜結(jié)果。你們的回復(fù)也沒有解釋為什么選擇性使用色譜分析結(jié)果。 Your system suitability test requires that … injections of standard be performed and that a Relative Standard Deviation (RSD) of … % be met in order for the test to be acceptable. This acceptance criterion is contrary to the USP requirement chapter <621>. During our inspection, you were unable to provide validation data to support your current RSD criteria. Your response is inadequate in that you failed to provide scientific rationale to justify the change in your analytical method for system suitability requirements. In response to this letter, please provide a valid % RSD and the analytical data to support it.你們的系統(tǒng)適用性實(shí)驗(yàn)要求…注射標(biāo)準(zhǔn)液計(jì)算RSD以符合接受標(biāo)準(zhǔn)，這個(gè)接受標(biāo)準(zhǔn)與USP通用要求<621>相反。在我們檢查期間，你們不能提供驗(yàn)證數(shù)據(jù)來支持你們當(dāng)前的RSD接受標(biāo)準(zhǔn)。你們的回復(fù)是不充分的，沒有提供科學(xué)的依據(jù)證明變更方法的系統(tǒng)適用性實(shí)驗(yàn)要求。在這個(gè)回復(fù)信中請(qǐng)你們提供有效證的RSD和分析數(shù)據(jù)來支持。 |
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