β-烟酰胺单核苷酸跨境产品中NMN含量的测定

Determination of β-Nicotinamide Mononucleotide(NMN) in NMN Cross Border Products

本文基于高效液相色谱法,通过优化色谱条件和样品前处理条件,建立了一种测定β-烟酰胺单核苷酸(NMN)胶囊和NMN片剂基质中NMN含量的检测方法,并进行方法学验证。结果表明,本方法在5~500μg/mL范围内有较好的线性关系,方法检出限(LOD,S/N=3)为1.0 mg/kg,定量限(LOQ,S/N=10)为3.0 mg/kg,仪器精密度为0.3%。对于NMN片剂样品,方法稳定性为1.7%,重复性为1.8%;对于NMN胶囊样品,方法稳定性为0.6%,重复性RSD值0.6%。NMN片剂和NMN胶囊样品中NMN的检测回收率在90.9%~108.9%之间,相对标准偏差均不超过1.9%。综上,本方法具有较好的重现性、精密度、稳定性、重复性,结果准确可靠,可用于实际样品中NMN含量的准确测定。通过对6种市售的NMN产品进行检测,所有样品中均检出了NMN,但是部分产品的实际含量较其标称含量偏少,发现部分产品存在虚报NMN含量的问题。本文研究为制定NMN跨境产品中NMN含量的检测方法标准奠定了方法学基础,对于提高NMN相关产品质量,促进相关产业的便捷监管具有深远意义。

By optimizing the chromatographic conditions and sample pretreatment conditions, a method for determination of NMN content in NMN capsules and NMN tablets matrix was established based on high performance liquid chromatography, and the methodology was verified. The results showed that, the method with range of 5~500 μg/mL had a good linear relationship. The limit of detection(LOD, S/N=3) of NMN was 1.0 mg/kg, while the limit of quantitative(LOQ,S/N=10) was 3.0 mg/kg. The precision of the instrument was 0.3%. For NMN tablet samples, the stability of the method was 1.7% and the repeatability was 1.8%, while for NMN capsule samples, the stability of the method was 0.6%, and the repeatability RSD value was 0.6%. The recovery of NMN in NMN tablets and NMN capsules was between 90.9% and108.9% with the RSD all no more than 1.9%. In conclusion, this method had good reproducibility, precision, stability and repeatability, could give accurate and reliable results, and could be used for the accurate determination of NMN in actual samples. Through the detection of 6 kinds of commercially available NMN products, NMN was detected in all samples, but the actual contents of some products were less than their nominal content. It was found that some products had the problem of false reporting of NMN content. This study would lay a methodological foundation for formulating the detection method standard of NMN content in NMN related dietary supplement products, and was of far-reaching significance for improving the quality of NMN related products and promote the convenient supervision of related industries.