二丁酰环磷腺苷钠的制备及其含量和相关物质的测定

Preparation of sodium dibutyryladenosine cyclophosphate and the determination of the content and related substances

目的 制备二丁酰环磷腺苷钠并测定其含量及有关物质.方法 自制二丁酰环磷腺苷钠后,采用高效液相色谱法测定其含量和有关物质,色谱条件为：ODS C18柱（4.6 mm×250 mm,5μm）,以乙腈-0.05 mol/mL磷酸二氢钾溶液（25∶75）为流动相,流速1 mL/min,273 nm为检测波长.结果 二丁酰环磷腺苷钠为白色粉末状固体（收率＞70％,HPLC＞ 99％）;含量测定线性范围为20～30μg/mL,r=0.9997;重复性良好（RSD=0.4％,n=6）;回收率为101.2％（RSD =0.3％）;有关物质定量限为50.08 ng/mL,该浓度下检测结果稳定;线性范围为0.05 ～ 3.75 μg/mL,r=0.9999;重复性良好（RSD=4.53％,n=6）;回收率为93.5％（RSD =1.8％）.结论 该合成路线简单,制备得到二丁酰环磷腺苷钠纯度高,建立的HPLC法测定其含量及有关物质简便,结果可靠.

Objective To prepare sodium dibutyryladenosine cyclophosphate（ dbc AMP-Na）,and determine the content and related substances.Methods Determine the content and related substances of dbc AMP-Na by high performance liquid chromatography after prepared,The column： ODS C18column（ 4. 6 mm × 250 mm,5 μm）; the mobile phase： acetonitrile-0. 05 mol / m L Ka H2PO4solution（ 25 ∶75）; the flow rate： 1 m L / min; the content of dbc AMP-Na was detected at 273 nm. Results The linear range of the determination of the content was 20 ~ 30 μg / m L,and the correlation coefficient was0. 9997; The precision was good（ RSD = 0. 4%,n = 6）; The recovery result was 101. 2%（ RSD = 0. 3%）. The quantitative limit of relevant material is50. 08 ng / m L,which is stable under this concentration; The linear range of the determination was 0. 05 ~ 3. 75 μg / m L,r = 0. 9999; The precision was good（ RSD = 4. 53%,n = 6）; The recovery result was 93. 5%（ RSD = 1. 8%）. Conclusion The synthetic route of dbc AMP-Na is simple and with high product purity. The method to determine the content and related substances of dbc AMP-Na is easy to operate and the results of the determination are accurate.