辣椒油中罂粟碱标准样品的制备与定值

Preparation and determination of papaverine standard samples in chili oil

制备辣椒油基质中罂粟碱分析标准样品。在辣椒油样品中加入一定浓度和比例的盐酸罂粟碱标准品,振荡混匀后定量分装,密封避光保存。随机抽取15个独立包装的样品进行均匀性检测,采用单因素方差分析法(F检验)对样品的均匀性进行检验;同时开展短期稳定性和长期稳定性检验,通过F检验和回归统计分析进行样品稳定性检验,并由9个有资质的实验室采用液相色谱-串联质谱法协同定值。通过分析标准样品制备过程中的不确定度来源,计算不确定度分量、合成标准不确定度及扩展不确定度。制备的辣椒油中罂粟碱标准样品均匀性、稳定性良好,罂粟碱含量(质量分数)为(39.4±3.0)μg/kg(k=2)。所制备的标准样品可用于火锅食品系列中罂粟碱检测的方法验证和质量控制。

The standard sample was prepared for analysis of papaverine in pepper oil matrix.A certain concentration and proportion of papaverine hydrochloride standard was added to the samples of chili oil,which was mixed by shaking,quantitatively packed,sealed and stored away from light.Fifteen independently packaged samples were randomly selected for homogeneity detection,and one-way analysis of variance(F-test)was used to process the homogeneity of the samples.At the same time,the stability tests of short-term and long-term were carried out,and the results were evaluated by F-test and regression statistical analysis,and coordinated the value by 9 qualified laboratories used liquid chromatoc-tandem mass spectrometry.By analyzing the source of uncertainty in the preparation of standard samples,the uncertainty component,synthetic standard uncertainty and extended uncertainty were calculated.The prepared standard sample of papaverine in chili oil had good uniformity and stability,and the papaverine content was(39.4±3.0)μg/kg(k=2).The standard samples can be used for the verification and quality control of papaverine in hot pot food series.