USP〈1225〉药典规程的验证(中英文对照)(11)

For instrumental procedures, the same approach may be used as for non-instrumental procedures. In the case of procedures submitted for consideration as official compendial procedures, it is almost never necessary to determine the actual detection limit. Rather, the detection limit is shown to be sufficiently low by the analysis of samples with known concentrations of analyte above and below the required detection level. For example, if it is required to detect an impurity at the level of 0.1%, it should be demonstrated that the procedure will reliably detect the impurity at that level.

对于仪器分析规程，可以使用与非仪器分析规程相同的方法。对于提交用于官方药典规程的备选方法，其几乎从来不需要确定实际的检测限度。而是，通过分析含有高于和低于必需的检测水平的、已知待分析物浓度的样品，以显示检测限度足够低。例如，如果必需检测浓度在0.1%的杂质，则应当证明该分析规程将可靠地检测在这个水平的杂质。

In the case of instrumental analytical procedures that exhibit background noise, the ICH documents describe a common approach, which is to compare measured signals from samples with known low concentrations of analyte with those of blank samples. The minimum concentration at which the analyte can reliably be detected is established. Typically acceptable signal-to-noise ratios are 2:1 or 3:1. Other approaches depend on the determination of the slope of the calibration curve and the standard deviation of responses. Whatever method is used, the detection limit should be subsequently validated by the analysis of a suitable number of samples known to be near, or prepared at, the detection limit.

对于展示出背景噪音的仪器分析规程，ICH文件描述了一个通用方法，用来比较从以下样品测得的信号，这些样品分别为含已知低浓度被分析物的样品和空白样品。这样就确立了能够可靠检测的待分析物的最低浓度。可接受的典型信噪比是2:1或3:1。其他方法取决于校正曲线斜率的测定和响应值的标准差。无论用什么方法，均应该在随后通过分析适当数量的、已知接近或制备于检测限度的样品，来验证检测限度。

QUANTITATION LIMIT定量限度

Definition---- The quantitation limit is a characteristic of quantitative assay for low levels of compounds in sample matrices, such as impurities in bulk drug substances and degradation products in finished pharmaceuticals. It is the lowest amount of analyte in a sample that can be determined

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