摘要
目的:建立同时测定盐酸阿糖胞苷原料药的含量和有关物质的方法。方法:采用超高效液相色谱法。色谱柱为Inertsil ODS-3 C18流动相为磷酸盐缓冲液-甲醇(梯度洗脱),流速为0.8ml/min,检测波长为254nm,柱温为40℃,进样量为10μl。结果:尿嘧啶、尿苷、阿糖尿苷、盐酸阿糖胞苷检测质量浓度分别在0.1008~20.16、0.1~20.12、0.0956~19.12、0.1~20.004μg/ml范围内与各自峰面积积分值呈良好的线性关系(r=0.9999、0.9998、0.9999、0.9999);精密度、稳定性、重复性试验的RSD≤0.79%;尿嘧啶、尿苷、阿糖尿苷平均加样回收率为103.8%、102.2%、99.7%,RSD分别为2.44%、2.69%、3.16%(n=9)。结论:该方法准确、灵敏度高、专属性强、重复性好.可用于盐酸阿糖胞苷原料药的质量控制。
OBJECTIVE: To establish a method for simultaneous determination of cytarabine hydrochloride and related substance. METHODS: UPLC method was adopted. The determination was performed on Inertsil ODS-3 CIS column with mobile phase consisted of phosphate buffer-methanol (gradient elution) at the flow rate of 0.8 ml/min; the detection wavelength was set at 254 nm and the column temperature was 40℃. The sample size was 10μl. RESULTS: The liner ranges were 0.100 8-20.16 μg/ml for uracil (r=0.999 9), 0.1-20.12 μg/ml for uridine (r=0.999 8), 0.0956-19.12 ug/ml for 1-β-D-arabino furanosyl-uracil (r=0.999 9) and 0.1-20.004 μg/ml for cytarabine hydrochloride (r=0.999 9), respectively. RSD of precision, stability and reproducibility tests were all lower than 0.79%; average recoveries of uracil, wridine and 1-β-D-arabino furanosyl-uracil were 103.8% (RSD=2.44%, n=9), 102.2% (RSD=2.69%, n=9) and 99.7% (RSD=3.16%, n=9). CONCLUSIONS: The method is accurate, sensitive, specific and reproducible, and can be used for the quality control of cytarabine hydrochloride.
出处
《中国药房》
CAS
CSCD
2014年第12期1137-1140,共4页
China Pharmacy
关键词
盐酸阿糖胞苷
尿嘧啶
尿苷
阿糖尿苷
超高效液相色谱法
含量测定
Cytarabine hydrochloride
Uracil
Uridine
1-β-D- arabino furanosyl -uracil
UPLC
Content determination