中药陈皮提取物粉末中糊精含量近红外分析方法的验证和不确定度评估

目的：建立陈皮提取物粉末中辅料糊精含量近红外定量的方法验证和不确定度计算的全局评价策略。方法：通过采集已知不同含量糊精和陈皮混合样品的近红外光谱信息，建立偏最小二乘模型（PLS），基于β-容度容忍区间（β-CTI）建立准确度曲线对近红外（near infrared，NIR）分析方法进行验证，并通过β-CTI进行不确定度评估。结果：浓度水平为1%、3%、5%时，分析方法的准确度在可接受范围之外，该方法不可接受；浓度水平为7%和10%时，分析方法的准确度在可接受范围之内，该方法可以接受。所建NIR分析方法的最低定量限约等于5.73%。不确定度评估表明该方法在浓度较高时，方法的不确定度较好。结论：通过引入β-CTI同时进行方法验证和不确定度计算的全局评价策略可以有效保障方法的可靠性和准确性，有效降低分析方法在日常应用中的风险，为其他分析方法的评价提供借鉴。

Objective: To establish an overall evaluation strategy for the validation and uncertainty evaluation of near infrared(NIR)quantification of dextrin in dried tangerine.Methods: Through collecting the NIR spectral information of mixed samples with different contents of dextrin in dried tangerine, the NIR quantitative PLS model was built. Based on the β-content tolerance interval(β-CTI), the accuracy profile(AP)was established to validate the NIR analytical method and the uncertainty was also evaluated by the β-CTI.Results: When the dextrin content was 1%, 3%, 5% the accuracy was beyond acceptable limit and the method is unacceptable; When the dextrin content was 7%, 10% the accuracy was within acceptable limit and the method is acceptable. The lower limit of quantification(LLOQ)of the method was approximately equal to 5.73%. Uncertainty evaluation showed that the method had a good uncertainty at higher contents.Conclusion: The overall evaluation strategy for validation and uncertainty assessment at the same time through the introduction of β-CTI can ensure the reliability and accuracy of method, reduce the risk of method in the daily use, and provide reference for the evaluation of other analytical methods.

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