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目的对制备的高纯脱水河豚毒素(Anh-TTX)样品进行结构验证与毒力测定。方法采用LC-FLD检测法分析Anh-TTX样品纯度,采用MS和~1H NMR对样品进行结构验证;进行高纯Anh-TTX对小鼠的LD_(50)测定。结果Anh-TTX样品纯度为98.3%,样品MS图谱信息与Anh-TTX的结构完全相符,~1H NMR数据与文献报道值基本一致;测得高纯Anh-TTX对小鼠的LD_(50)为(1862±6)μg·kg~(-1)。结论Anh-TTX样品的纯度高,得到MS和~1H NMR的确证。Anh-TTX对小鼠有较强毒性,但毒力远低于河豚毒素(TTX)。
OBJECTIVE To investigate the structure and toxicity of prepared Anh-TTX samples. Methods The purity of Anh-TTX was determined by LC-FLD. The structure of Anh-TTX was confirmed by MS and 1H NMR. LD_ (50) was determined by high purity Anh-TTX in mice. Results The purity of Anh-TTX sample was 98.3%. The MS spectrum of the sample was completely consistent with the structure of Anh-TTX. The 1H NMR data were consistent with those reported in the literature. The LD 50 of the purified Anh-TTX was (1862 ± 6) μg · kg -1. Conclusion The purity of Anh-TTX sample is high and confirmed by MS and 1H NMR. Anh-TTX is more toxic to mice, but virulence is much lower than that of tetrodotoxin (TTX).