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发表于 2013-6-27 21:33:10
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6. DETECTION LIMIT Several approaches for determining the detection limit are possible, depending on whether the procedure is a non-instrumental or instrumental. Approaches other than those listed below may be acceptable. 6.1. Based on Visual Evaluation Visual evaluation may be used for non-instrumental methods but may also be used with instrumental methods. The detection limit is determined by the analysis of samples with known concentrations of analyte and by establishing the minimum level at which the analyte can be reliably detected. 6.2. Based on Signal-to-Noise This approach can only be applied to analytical procedures which exhibit baseline noise. Determination of the signal-to-noise ratio is performed by comparing measured signals from samples with known low concentrations of analyte with those of blank samples and establishing the minimum concentration at which the analyte can be reliably detected. A signal-to-noise ratio between 3 or 2:1 is generally considered acceptable for estimating the detection limit. 6.3 Based on the Standard Deviation of the Response and the Slope The detection limit (DL) may be expressed as: DL = 3.3 σ S where σ = the standard deviation of the response S = the slope of the calibration curve The slope S may be estimated from the calibration curve of the analyte. The estimate of σ may be carried out in a variety of ways, for example: 6.3.1 Based on the Standard Deviation of the Blank Measurement of the magnitude of analytical background response is performed by analyzing an appropriate number of blank samples and calculating the standard deviation of these responses. 6.3.2 Based on the Calibration Curve A specific calibration curve should be studied using samples containing an analyte in the range of DL. The residual standard deviation of a regression line or the standard deviation of y-intercepts of regression lines may be used as the standard deviation. 6.4 Recommended Data The detection limit and the method used for determining the detection limit should be presented. If DL is determined based on visual evaluation or based on signal to noise ratio, the presentation of the relevant chromatograms is considered acceptable for justification.
In cases where an estimated value for the detection limit is obtained by calculation or extrapolation, this estimate may subsequently be validated by the independent analysis of a suitable number of samples known to be near or prepared at the detection limit. |
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