摘要
目的对红花注射液中核苷类成分进行研究。方法 采用液质联用技术(LC-MS),以乙腈-0.05%三氟乙酸溶液为流动相梯度洗脱,以Phenomenex Gemini-C18色谱柱为分析柱,通过电喷雾电离源(ESI),选择正离子模式全扫描方式检测,对红花注射液中核苷类成分进行分析鉴定。采用超高效液相色谱(UPLC),以0.05%三氟乙酸溶液为流动相,ACQUITY UPLC HSS T3色谱柱为分析柱,流速0.4 mL.min-1,检测波长260 nm,柱温40℃,对所鉴定的核苷类成分进行含量测定。结果 红花注射液中检测到腺苷、鸟苷、尿苷和胞苷4种核苷成分。UPLC测定4种核苷成分在选定的范围内线性关系良好(r≥0.999 7),平均回收率在99.0%～101.4%,RSD<1.5%(n=6)。市售18个批次红花注射液中上述4种核苷成分含量分别分布在0.033～0.162,0.008～0.052,0.048～0.184,0.031～0.064 mg·mL-1。结论红花注射液中含有4种核苷类成分,其中腺苷和尿苷含量较高,但不同企业之间含量存在较大差异。
OBJECTIVE To study nucleosides in Safflower injection. METHODS Nucleosides in Safflower injection were identified by LC-MS. The separation was performed on Phenomenex Gemini-C18 column. Gradient elotion was carried out with mobile phase consisting of acetonitrile-0. 05% trifluoroacetic acid. Electrospray ionization source was applied and operated in the positive ion mode. Four nucleosides in Safflower injection were simultaneously determined by ultra performance liquid chromatography （UPLC） with AC- QUITY UPLC HSS T3 column. The mobile phase was 0. 05% trifluoroacetic acid aqueous solution at the flow rate of 0. 4 mL min-L. The assay was carried out at 40 ℃ with detection at 260 nm. RESULTS Adenosine, guanosine, uridine and cytidine in safflower injection were identified. The relationship between the injection quality and the peak areas of the four nucleosides was all linear. The average recoveries （n =6） were in the range of 99. 0% - 101.4% and the RSDS were all less than 1.5%. The contents of the four nucleosides in tested samples were in the field of 0. 033 -0. 162,0. 008 -0. 052,0. 048 -0. 184 and 0.031 -0. 064 mg . mL^-1. CONCLUSION There are four nucleosides in safflower injection. The contents of adenosine and uridine are relatively high. There was sig- nificant difference in the contents of the tested samples.
出处
《中国药学杂志》
CAS
CSCD
北大核心
2013年第12期1022-1026,共5页
Chinese Pharmaceutical Journal
