固体复合香辛料中罂粟壳质控样的制备

Preparation of Quality Control Sample for Poppy Shell in Solid Compound Spice

建立了一种固体复合香辛料中罂粟壳质控样制备方法。将香辛料基质材料与罂粟壳各自经微波干燥、混合、粉碎和过筛,后经一次混合、加抗结剂、二次干燥、二次过筛和二次混合后,制得200份质控样本。经均匀性与稳定性检验后,由10家实验室采用液相色谱-串联质谱法对样本进行协同定值,并进行不确定度评估。结果表明:样本中5种生物碱类物质的特性值分别为可待因(907±20.9)μg/kg,蒂巴因(918±18.4)μg/kg,吗啡(315±16.5)μg/kg,罂粟碱(171±12.6)μg/kg,那可丁(139±15. 8)μg/kg,均匀性与稳定性良好,适用于复合香辛料中生物碱类物质检测过程的方法验证与质量控制。

To establish a method for quality control samples for the poppy shell in solid compound spices.The spice matrix materials and the poppy shell were dried by microwave,mixed,pulverized,sieved,and then mixed again.After added with antagonist,the samples were dried,sieved,and mixed again.The homogeneity and stability of the samples were strictly examined.The concentrations of each chemical constituent in the samples were collaboratively analyzed using liquid chromatography-tandem mass spectrometry in 10 laboratories and then the uncertainty was assessed.The results showed that the characteristic values of the codeine,thebaine,morphine,papaverine,noscapine in these samples were(907±20.9),(918±18.4),(315±16.5),(171±12.6),(139±15.8)μg/kg respectively.The uniformity and stability was good.The methodology is suitable for verifying alkaloids in solid compound spices to control the quality.