纯化纳米雄黄制备方法探讨

Preparation of purified realgar nanoparticles

目的探讨纯化纳米雄黄的制备方法,以制备高纯度、高生物利用度、低毒副作用的纯化纳米雄黄颗粒。方法①天然雄黄经去离子水和不同浓度的HCl、NaOH纯化处理后得到纯化雄黄,测定As2S2含量;②天然雄黄、纯化雄黄经高能球磨法制备得到天然纳米雄黄、纯化纳米雄黄,颗粒经扫描电镜、纳米粒度分析仪测定纳米颗粒形貌、粒径,测定As2S2含量;③天然纳米雄黄、纯化纳米雄黄经2.0 mol·L-1的HCl纯化处理得到天然纳米雄黄(纯化组)、纯化纳米雄黄(纯化组),扫描电镜、纳米粒度分析仪测定纳米颗粒形貌、粒径;测定As2S2含量。结果①去离子水;0.5、1.0、2.0、4.0 mol·L-1的HCl与NaOH纯化处理后颗粒As2S2含量均有所提高,各处理组之间差异有统计学意义(P<0.05);纯化效果:HCl组>NaOH组>去离子水组,随着HCl、NaOH浓度的提高,As2S2的含量亦随之提高;以4.0 mol·L-1 HCl组纯化效果最显著,其次为2.0 mol·L-1HCl组。②天然雄黄、纯化雄黄、天然纳米雄黄(纯化组)、纯化纳米雄黄(纯化组)经高能球磨法可制备得到纳米级雄黄颗粒,扫描电镜可见近似圆球形的纳米级颗粒,粒度分布均匀,纳米粒度分析仪测定其平均粒度分别为(135.13±9.19)、(134.39±4.57)、(135.88±2.68)、(133.73±4.36)nm;As2S2含量分别为(92.09±0.83)%、(97.07±0.47)%、(97.42±0.11)%、(98.33±0.08)%。纳米雄黄组与纳米雄黄(纯化组)粒度差异无统计学意义(P>0.05),纯度差异有统计学意义(P<0.05)。结论①去离子水、HCl、NaOH均可对雄黄进行纯化处理,以HCl纯化效果为最好;②高能球磨法可制备纳米雄黄颗粒;③球磨前后分别对雄黄颗粒进行纯化处理,可得到As2S2含量更高的纯化纳米雄黄颗粒。

Objective To prepare purified realgar nanoparticles, which have higher purity, higher bioavailability and fewer side effects. Methods ① Crude realgar was purified by distilled water, different concentrations of hydrochloric acid（HCl） and sodium hydroxide（NaOH）, then the content of arsenic disulfide（As2S2） measured. ② Crude realgar nanoparticles and purified realgar nanoparticles were prepared by high-energy ball milling technology, the average size and the shape of particles were determined by nanoparticle size analyzer and scanning electron microscopy, and the content of As2S2 measured. ③ Crude realgar nanoparticles（purified group）, and purification realgar nanoparticles（purified group） were handled by 2.0 mol·L- 1 HCl, the average size and the shape of particles were determined by scanning electron microscopy, nanoparticle size analyzer, and then the content of As2S2 measured. Results ① The distilled water, 0.5, 1.0, 2.0, 4.0 mol·L- 1 of the HCl and NaOH increased the content of As2S2. There was significant difference among the treatment groups（P 0.05）; the HCl group had most purification effect, followed by NaOH group and distilled water group. With the increase of HCl and NaOH concentration, the content of As2S2 also improved, and the 4.0 mol·L- 1 HCl group had the most purification effect, followed by 2.0 mol·L- 1 HCl. ② The nanoparticles of crude realgar, the purified realgar, crude realgar nanoparticles（purified group）, and purified realgar nanoparticles（purified group） were prepared by high-energy ball milling technology. By scanning electron microscopy, the nanoparticles were approximately spherical and the particles size distribution was average. The nanoparticle size analyzer measured the average particle size at（135.13±9.19）,（134.39±4.57）, and（135.88±2.68）,（133.73±4.36） nm, and the As2S2 contents were（92.09±0.83）%,（97.07±0.47）%,（97.42±0.11）%, and（98.33±0.08）%. From particle size aspect, nanoparticles realgar group and nanoparticles realgar（purified group） had no statistical significance（P 0.05）, but in the purification aspect, there was statistical significance（P 0.05）. Conclusion ① Crude realgar can be purified by distilled water, HCl and NaOH, and the HCl group has the best purification effect. ② Nanoparticles realgar can be prepared by high-energy ball milling technology. ③ Before and after ball milling process, we can obtain purified realgar nanoparticles.