纳米雄黄炮制方法的探讨

目的:以炮制品得率及残渣质量,粒径分布,As2S2和As2O3的含量为指标,考察不同炮制方法对纳米雄黄的影响,筛选其最佳炮制方法。方法:采用高能球磨法制备纳米雄黄生品,利用水飞法、酸水飞法和碱水飞法对其进行炮制,计算各炮制品得率及残渣质量;利用激光散射法测定粉体粒径,电镜扫描法观察粉体的表观形貌;直接碘量法和二乙基二硫代氨基甲酸银法(Ag-DDC法)分别测定各样品中As2S2与As2O3的含量。结果:水飞品、酸水飞品和碱水飞品的得率分别为96.71%,95.86%,79.08%,残渣质量分别为0.328,0.891,2.208 g;生品及各炮制品的平均粒径分别为(157.3±4.8),(143.9±6.2),(137.7±4.5),(139.8±5.3)nm;As2S2质量分数分别为(94.26±1.33)%,(98.97±0.98)%,(99.58±1.45)%,(99.37±2.60)%,As2O3质量分数分别为(9.64±0.68),(3.44±0.29),(2.83±0.27),(18.17±1.70)mg·g-1。结论:3种炮制方法均能减小纳米雄黄生品的粉体粒径,提高其As2S2的含量,且水飞法和酸水飞法均可降低其As2O3的含量。确定最佳炮制方法为酸水飞法。

Discussion of Processing Methods of Nano-Realgar

Objective: To investigate the effect of different processing methods on nano-Realgar for screening the best processing methods,with processed products yield,weight of the residue,particle size distribution and the contents of As₂S₂ and As₂O₃ as indicators. Method: Raw products of nano-Realgar were prepared by high-energy ball milling technology and processed by water,acid water and alkali water,then calculated the yield of processed products and the weight of residue.The average size and the morphology of particles were determined by laser scattering analyzer and scanning electron microscopy (SEM).And the contents of As₂S₂ and As₂O₃ in different samples were detected by direct iodine titration method and silver diethyl dithiocarbamate (Ag-DDC) method,respectively. Result: Yields of processed products by water,acid water and alkali water were 96.71%,95.86% and 79.08%,the weights of residue were 0.328,0.891,2.208 g.The average sizes of raw products and processed products by water,acid water and alkali water were (157.3±4.8),(143.9±6.2),(137.7±4.5),(139.8±5.3) nm,contents of As₂S₂ of them were (94.26±1.33)%,(98.97±0.98)%,(99.58±1.45)% and (99.37±2.60)%,contents of As₂O₃ were (9.64±0.68),(3.44±0.29),(2.83±0.27),(18.17±1.70) mg·g^-1. Conclusion: These three kinds of processing methods can reduce the average particle size of raw products of nano-Realgar and improve the content of As₂S₂.In addition,the water and acid water method can both reduce the content of As₂O₃ in raw products of nano-Realgar.The acid water processing is the best.