{"id":59941,"date":"2018-10-29T01:00:00","date_gmt":"2018-12-07T02:51:49","guid":{"rendered":"http:\/\/www.05921.net\/index.php\/2018\/12\/07\/a1bf84bfa3\/"},"modified":"2018-12-07T10:52:08","modified_gmt":"2018-12-07T02:52:08","slug":"a1bf84bfa3","status":"publish","type":"post","link":"https:\/\/www.05921.net\/index.php\/59941\/","title":{"rendered":"PDA TR 80\uff1a\u624b\u52a8\u79ef\u5206\u6307\u5357\u3001\u5ba1\u8ba1\u8ddf\u8e2a\u4ee5\u53ca\u7535\u5b50\u6570\u636e\u7ba1\u7406\u7b49"},"content":{"rendered":"
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\"PDA<\/p>\n

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Data Processing and Peak Integration
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\u6570\u636e\u5904\u7406\u548c\u5cf0\u7684\u79ef\u5206<\/strong><\/span><\/p>\n


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Chromatographic software uses dynamic peak detection algorithms and automatic peak detection algorithms. Integrating the chromatograms using software to apply the integration events, such as peak width, threshold, height, and area, etc., and then visually observing the peak integration for its correctness is generally recommended. The inherent or analytical variations and combination of various and drifting baselines in which the auto-integration will either underreport or overintegrate the peak areas.<\/p>\n

\u8272\u8c31\u8f6f\u4ef6\u4f7f\u7528\u52a8\u6001\u5bfb\u5cf0\u7b97\u6cd5\u548c\u81ea\u52a8\u5bfb\u5cf0\u7b97\u6cd5\u3002\u901a\u5e38\u5efa\u8bae\u5148\u7528\u8f6f\u4ef6\u79ef\u5206\u8272\u8c31\u6765\u5904\u7406\u50cf\u5cf0\u5bbd\u3001\u9608\u503c\u3001\u5cf0\u9ad8\u53ca\u5cf0\u9762\u79ef\u7b49\u9700\u8981\u79ef\u5206\u7684\u60c5\u5f62\uff0c\u518d\u4eba\u5de5\u786e\u5b9a\u79ef\u5206\u7684\u6b63\u786e\u6027\u3002\u56e0\u4e3a\u4e00\u4e9b\u56fa\u6709\u7684\u6216\u5206\u6790\u53d8\u5316\u6216\u4e24\u8005\u7686\u6709\u4ee5\u53ca\u57fa\u7ebf\u6f02\u79fb\u7684\u539f\u56e0\uff0c\u81ea\u52a8\u79ef\u5206\u5c06\u4f1a\u4f7f\u5cf0\u9762\u79ef\u504f\u5927\u6216\u8005\u504f\u5c0f\u3002<\/span><\/p>\n


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Once acquired, the electronic raw data of the measurements (measured values and metadata) are stored and available for processing. Some acquired electronic raw data already represent usable results (e.g., weight, temperature, and humidity). Other acquired electronic raw data, such as intensity values correlated with time or wavelength and generated by chromatography or spectroscopy, require further processing to obtain usable results (e.g., retention times, peak areas, and amounts). These processes, such as integration and calibration, are defined by processing parameters or calibration factors and affect only the resultant data after processing, but not the acquired electronic raw data. In contrast to the acquired electronic raw data, the processing parameters, such as integration events and calibration curves, may be changed during data evaluation. The changed processing parameters, methods, and processed data should be identified by versioning (i.e., number of times reprocessed) either on the results or from the audit trail data (25).<\/p>\n

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Integration events should be defined through standard algorithms, and metadata and should be associated with respective raw data files. In such cases, the analyst adjusts the integration events to obtain proper peak integration. As chromatography is a comparative technique, the consistent integration events should be applied for the entire set of chromatograms, as much as possible, or published along with the chromatograms. Figure 6.3.7-1 represents an overlaid chromatogram of the standard and a sample (of the same concentration) integrated with the same integration events. Integrating small peaks, closer peaks, negative peaks, drifting peaks, and peak-to-valley requires time and skill. Integrating peaks manually is not recommended and should be avoided to the extent possible.<\/p>\n

\u79ef\u5206\u4e8b\u4ef6\u5e94\u8be5\u901a\u8fc7\u6807\u51c6\u7b97\u6cd5\u548c\u5143\u6570\u636e\u8fdb\u884c\u5b9a\u4e49\uff0c\u4e14\u5904\u7406\u540e\u7684\u7ed3\u679c\u5e94\u4e0e\u5404\u81ea\u7684\u539f\u59cb\u6587\u6863\u8fdb\u884c\u5173\u8054\u3002\u53ea\u6709\u8fd9\u6837\uff0c\u5206\u6790\u5e08\u624d\u53ef\u4ee5\u901a\u8fc7\u8c03\u6574\u79ef\u5206\u4e8b\u4ef6\u4ece\u800c\u83b7\u5f97\u9002\u5f53\u7684\u5cf0\u9762\u79ef\u79ef\u5206\u3002\u56e0\u4e3a\u8272\u8c31\u662f\u4e00\u79cd\u6bd4\u5bf9\u6280\u672f\uff0c\u6240\u4ee5\u5e94\u5c3d\u53ef\u80fd\u7684\u5c06\u540c\u4e00\u79ef\u5206\u4e8b\u4ef6\u5e94\u7528\u4e8e\u6574\u4e2a\u8272\u8c31\u56fe\u96c6\u6216\u548c\u6574\u4e2a\u8272\u8c31\u56fe\u4e00\u8d77\u53d1\u5e03\u3002\u56fe 6.3.7-1\u8868\u793a\u6807\u51c6\u54c1\u548c\u67d0\u6d53\u5ea6\u4e0b\u7684\u6837\u54c1\u901a\u8fc7\u540c\u6837\u7684\u79ef\u5206\u4e8b\u4ef6\u8fdb\u884c\u79ef\u5206\uff0c\u5e76\u4e00\u540c\u5448\u73b0\u5728\u540c\u4e00\u8272\u8c31\u56fe\u4e2d\u3002\u5bf9\u5c0f\u5cf0\u3001\u63a5\u8fd1\u5cf0\u3001\u8d1f\u5cf0\u3001\u6f02\u79fb\u5cf0\u4ee5\u53ca\u5cf0\u8c37\u8fdb\u884c\u79ef\u5206\u9700\u8981\u65f6\u95f4\u548c\u6280\u5de7\u3002<\/span>\u4e0d\u63a8\u8350\u624b\u52a8\u79ef\u5206\uff0c\u4e14\u5e94\u5c3d\u53ef\u80fd\u907f\u514d\u8fdb\u884c\u624b\u52a8\u79ef\u5206<\/span>\u3002<\/span><\/p>\n

\"PDA<\/p>\n


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QC laboratories should have procedures in place that require authorization to perform manual integration and for procedures to track such events to avoid unnoticed or unevaluated cases that may affect the accuracy of the results. PDA defines manual integration as a process used by a person to manually integrate the peak height or area by modifying the baseline of the chromatogram with use of chromatographic software. The conditions and circumstances when manual integration would be allowed should be predefined (e.g., complexity of the sample matrix). Generally, a good chromatographic data system would be able to render consistent and reliable baselines for an overwhelming majority of injections within a chromatographic run. When consistently bad chromatographic peaks and baseline issues are encountered, having good documentation should not be the only way to address the issue. In this circumstance, the goal should be to improve the system and ensure that the data generated is reliable and consistent.<\/p>\n

QC\u5b9e\u9a8c\u5ba4\u5e94\u5efa\u7acb\u9700\u8981\u6388\u6743\u624d\u80fd\u8fdb\u884c\u624b\u52a8\u79ef\u5206\u7684\u7a0b\u5e8f\u5e76\u8ffd\u8e2a\u6b64\u7c7b\u4e8b\u4ef6\uff08\u6ce8\uff1a\u624b\u52a8\u79ef\u5206\uff09\u7684\u7a0b\u5e8f\uff0c\u907f\u514d\u56e0\u4e3a\u4eba\u5458\u5ffd\u89c6\u6216\u8005\u672a\u8bc4\u4f30\u800c\u5f71\u54cd\u7ed3\u679c\u7684\u51c6\u786e\u6027\u3002PDA\u5c06\u624b\u52a8\u79ef\u5206\u5b9a\u4e49\u4e3a\uff1a\u7531\u4eba\u5458\u4f7f\u7528\u8272\u8c31\u8f6f\u4ef6\u4fee\u9970\u8272\u8c31\u56fe\u7684\u57fa\u7ebf\u6765\u4eba\u4e3a\u5bf9\u5cf0\u9ad8\u6216\u8005\u5cf0\u9762\u79ef\u8fdb\u884c\u79ef\u5206\u7684\u8fc7\u7a0b\u3002<\/span>\u5e94\u5f53\u4e8b\u5148\u5b9a\u4e49\u5141\u8bb8\u8fdb\u884c\u624b\u52a8\u79ef\u5206\u7684\u6761\u4ef6\u548c\u60c5\u5f62\uff08\u5982\uff1a\u590d\u6742\u7684\u6837\u54c1\u57fa\u8d28\uff09\u3002<\/span>\u901a\u5e38\uff0c\u4e00\u4e2a\u826f\u597d\u7684CDS\u7cfb\u7edf\u5e94\u8be5\u80fd\u591f\u5728\u8272\u8c31\u8fd0\u884c\u4e2d\u4e3a\u7edd\u5927\u591a\u6570\u8fdb\u9488\u63d0\u4f9b\u8fde\u7eed\u4e14\u53ef\u9760\u7684\u57fa\u7ebf\u3002\u5f53\u8272\u8c31\u5cf0\u8fde\u7eed\u6bd4\u8f83\u5dee\u4e14\u53d1\u751f\u57fa\u7ebf\u53d1\u751f\u95ee\u9898\u65f6\uff0c\u5c06\u95ee\u9898\u5b8c\u6574\u7684\u8bb0\u5f55\u4e0b\u6765\u5e76\u4e0d\u662f\u552f\u4e00\u7684\u89e3\u51b3\u9014\u5f84\u3002\u5728\u8fd9\u79cd\u60c5\u51b5\u4e0b\uff0c\u5e94\u8be5\u4ee5\u6539\u5584\u7cfb\u7edf\u5e76\u786e\u4fdd\u4ea7\u751f\u7684\u6570\u636e\u771f\u5b9e\u53ef\u4fe1\u4e3a\u76ee\u7684\u3002<\/span><\/p>\n


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The Quality Unit  should define standard protocols for processing data to include the following, which may be instrument or application-specific:<\/p>\n

\u8d28\u91cf\u90e8\u95e8\u5e94\u5b9a\u4e49\u5904\u7406\u6570\u636e\u7684\u6807\u51c6\u65b9\u6848<\/span>\uff0c\u53ef\u4ee5\u662f\u9488\u5bf9\u4eea\u5668\u6216\u7279\u5b9a\u5e94\u7528\u3002\u65b9\u6848\u5e94\u5305\u542b\u4ee5\u4e0b\u5185\u5bb9\uff1a<\/span><\/p>\n


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