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嘉峪檢測網 2022-08-01 08:03
近日,EDQM官網刊登了關于新版歐洲藥典通論2.2.46《色譜分離技術》修訂的公告,新的通論2.2.46《色譜分離技術》現已在《歐洲藥典》第11版(Ph. Eur. 11.0,)中提供,并將于2023年1月1日生效!
General chapter2.2.46. Chromatographic separation techniques has been revised to incorporate the provisions of the pharmacopoeial harmonisation text, signed-off by the Pharmacopoeial Discussion Group (PDG) on 28 September 2021. The revised chapter is now available in the 11th Edition of the Europe Pharmacopoeia (Ph. Eur. 11.0, implementation date: 1 January 2023).
《歐洲藥典》已對通論第2.2.46章《色譜分離技術》進行修訂,該章節由藥典討論小組(PDG)于2021年9月28日簽署。修訂后的章節現已在《歐洲藥典》第11版(Ph. Eur. 11.0,實施日期:2023年1月1日)中提供。
This general chapter applies to chromatographic analytical procedures and supplements the general chapters onThin-layer chromatography (2.2.7), Gas chromatography (2.2.28), Liquid chromatography (2.2.29) and Size-exclusion chromatography (2.2.30). In addition to definitions of chromatographic features, it contains system suitability requirements for LC and GC procedures, complementing those given in the individual monographs.
該章節適用于色譜分析程序,并補充了關于薄層色譜(2.2.7)、氣相色譜(2.2.28)、液相色譜(2.2.29)和尺寸排阻色譜(2.2.30)的通論。除了色譜特征的定義外,它還包含LC和GC程序的系統適用性要求,補充了各個各論中給出的要求。
The main changes made for harmonisation purposes are:
主要修改內容:
the signal-to-noise ratio is based on a baseline of 20 times the peak width at half height but if this is not obtainable, a baseline of at least 5 times the width at half-height is permitted;
信噪比基于半高時峰寬的20倍的基礎,但如果無法獲得,則允許半高處至少5倍峰寬的基礎;
the default symmetry factor range has been extended from 0.8-1.5 to 0.8-1.8; it applies to both tests and assays;
默認對稱因子范圍已從0.8-1.5擴展到0.8-1.8;它適用于檢查和含量測定;
the text now states that retention times and relative retentions are not requirements but are given for information in the monographs;
保留時間和相對保留不再在文中作出要求,而在各個專論中作為資料性信息;
the system repeatability requirement in the assay now applies to both active substances and excipients, with a target value of 100 per cent for a pure substance;
含量測定中的系統重復性要求現已適用于活性成分和輔料,純的成分的目標值為100%;
with regard to adjustments of chromatographic conditions, it is stressed that such adjustments are made only on the basis of the pharmacopoeial procedure. The fact that compliance with the system suitability test is always required (but is no longer the only factor prompting adjustments), that additional verification tests may be required when adjustments are made to a pharmacopoeial procedure and that multiple adjustments would trigger the need for a risk assessment is also clearly stated;
關于色譜條件的調整,需要強調的是,這種調整只是在藥典程序的基礎上進行的。還明確指出,始終需要符合系統適用性測試(但不再是允許色譜條件調整的唯一因素),在對藥典程序進行調整時可能需要額外的確認測試,并且多方面的調整會觸發風險評估的需要;
for liquid chromatography with isocratic elution, the harmonised conditions for adjustment of the stationary phase are stricter than in the former chapter; adjustments of column dimensions are now based on the L/dp ratio, as was already the case in United States Pharmacopeia (USP) chapter <621>, but with stricter requirements; harmonised conditions are also described for the adjustment of mobile phase composition, flow rate and injection volume;
對于具有等度洗脫的液相色譜,固定相調整的協調條件比前一版更嚴格;柱尺寸的調整現在基于L / dp比,就像美國藥典(USP)<第621章>中已經出現的情況一樣,但要求更嚴格;還描述了調整流動相組成、流量和進樣量的協調條件;
similar requirements and tolerances as for isocratic elution have been agreed for gradient elution in LC;
已就LC中的梯度洗脫達成了與等度洗脫類似的要求和公差;
in gas chromatography, the conditions for adjustment of the column dimensions, injection volume, split ratio, injection port and transfer-line temperatures (the latter two being new for Ph. Eur.) have been harmonised;
在氣相色譜中,調節色譜柱尺寸,進樣體積,分離比,進樣口和傳輸線溫度的條件(后兩者對于Ph. Eur.來說是新要求)已經協調;
the adjustments for supercritical fluid chromatography have been deleted as this technique is not used in any Ph. Eur. monographs.
超臨界流體色譜的調整已被刪除,因為該技術未在任何Ph. Eur.專論中使用。
As was the case in the former version of general chapter2.2.46, system sensitivity is to be checked on the basis of a minimum signal-to-noise ratio. This default requirement only applies to LC and GC tests (and not assays) for monographs that include a reporting threshold (or a disregard limit, in older monographs).
與原版通則2.2.46的情況一樣,系統靈敏度應根據最低信噪比進行檢查。此默認要求僅適用于包含報告閾值(或舊專著中的忽略限值)的各論的LC和GC測試(而不是測定)。
Local requirements, i.e. specific to an individual pharmacopoeia, will be placed between white diamonds (◊◊). For the Ph. Eur. chapter, these requirements include synonyms for retardation factors and guidance for determining the signal-to-noise ratio (e.g. solution to be used). Lastly, the term “relative retention time” or “RRT” will not be used in the Ph. Eur.
當地要求,即特定于單個藥典的要求,將被放置在白色(◊◊)之間。對于Ph. Eur.章節,這些要求包括延遲因子的同義詞和確定信噪比的指導(例如要使用的溶液)。最后,術語“相對保留時間”或“RRT”將不會在Ph. Eur中使用。
關于色譜條件的調整:
藥典上各品種項下的色譜條件,可以進行適當的調整,并滿足系統適用性的要求。目前,EP/USP/JP均對于色譜條件的調整作出了更細致和明確的要求,而當前中國藥典2020版,還沒有這樣的詳細描述。
中國藥典2020年版高效液相色譜法項下對調整的描述:
中國藥典2020年版氣相色譜法項下對調整的描述:
來源:GMP辦公室