硫酸氨基葡萄糖标准样品的研制

Development of Glucosamine Sulfate Certified Reference Material

研制了硫酸氨基葡萄糖标准样品。以盐酸氨基葡萄糖为原料,制备高纯硫酸氨基葡萄糖,采用红外光谱(IR)、高分辨质谱和核磁共振谱(NMR)进行结构确证。样品分装成200瓶样品后,采用高效液相色谱–蒸发光散射法进行均匀性检验、稳定性检验和定值分析。从样品中随机抽取15瓶进行均匀性检验,结果表明在95%的置信区间范围内样品均匀性良好。按照25℃长期试验稳定性(12个月)进行稳定性考察,结果表明在考察期间内样品稳定性良好。标准样品经国内8家具有分析资质的实验室进行协同定值,硫酸氨基葡萄糖标准样品定值结果为99.84%,相对扩展不确定度为0.18%(k=1.96)。该标准样品达到国家标准样品的技术要求,可用于有关硫酸氨基葡萄糖的分析方法校正和质量控制。

Glucosamine sulfate certified reference material was developed. Glucosamine sulfate was made from the glucosamine hydrochloride. The structure of glucosamine sulfate certified reference material was comfirmed by infrared spectroscopy （IR）, high resolution mass spectral （HRMS） and nuclear magnetic resonance （NMR）. The sample was divided into 200 bottles, the homogeneity and stability testing and quantitative analysis were carried out by high performance liquid chromatography with evaporative light-scattering detector （HPLC–ELSD）. According to analysis procedure of homogeneity, 15 bottles of sample were randomly taken from 200 bottles, and the resultswere validated byF-test statistical methods.The stability inspection was carried on the long-term（12 months）, and the results indicated that the period for glucosamine sulfate of storage was 12 months at 25℃. A cooperative certification was conducted with 8 qualified laboratories. The certified purity value of the reference material of glucosamine sulfate was 99.84% with a relative expaned uncertainty of 0.18%（k=1.96）. The reference material can conform to the technical requirement of the certified reference material. The material was intended for use in the method validation and quality control regarding glucosamine sulfate.