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机构地区:[1]浙江中医药大学,杭州310053 [2]浙江省食品药品检验研究院,杭州310004 [3]中美华东制药有限公司,杭州310011
出 处:《中国实验方剂学杂志》2015年第5期61-64,共4页Chinese Journal of Experimental Traditional Medical Formulae
基 金:国家"重大新药创制"科技重大专项(2012ZX09304-005)
摘 要:目的:建立HPLC同时测定百令胶囊中5种核苷类成分尿苷酸、尿苷、腺苷酸、鸟苷和腺苷含量的方法。方法:采用Ultimate AQ C18色谱柱(4.6 mm×250 mm,5μm),以甲醇-0.05 mol·L-1磷酸二氢钾溶液为流动相进行梯度洗脱,流速1.0m L·min-1,检测波260 nm,柱温25℃。结果:在该色谱条件下,尿苷酸、尿苷、腺苷酸、鸟苷和腺苷分离良好,且分别在35.25-528.8(r=1.000),38.07-571.1(r=1.000),34.96-524.5(r=0.999 8),38.34-575.1(r=1.000),39.84-597.6 ng(r=1.000)线性关系良好。加样回收率分别为101.2%,103.1%,96.7%,101.4%,103.2%,RSD分别为1.9%,1.1%,1.3%,2.7%,1.6%。结论:该HPLC含量测定方法结果准确、可靠,具有良好的专属性、精密度、重复性和稳定性,可用于百令胶囊的质量控制。Objective : To establish an HPLC method for simultaneous determination of five nucleosides, uridine 5'-monophosphate, uridine, adenosine 5'-monophosphate monohydrate, guanosine, adenosine in Bailing capsules. Method: The separation was developed on an Ultimate AQ C18 column (4.6 mm ×250 mm,5μm) by gradient elution with methanol-0.05 mol·L^-1 potassium dihydrogen phosphate solution, with flow rate at 1.0 mL·min-1 and column temperature at 25 ℃. The detection wavelength was at 260 nm. Result: The baseline separation of uridine 5'-monophosphate, uridine, adenosine 5'-monophosphate monohydrate, guanosine, and adenosine was successfully achieved. The results showed that these five ingredients had good linearity within the test ranges of 35.25-528.8 (r =1.000), 38.07-571.1 (r =1.000), 34.96-524.5 (r =0.999 8), 38.34-575. 1 (r=1.000) and 39.84-597.6 ng (r = 1.000), respectively. The recovery were 101.2% (RSD 1.9%), 103. 1% (RSD 1. life), 96.7% (RSD 1.3%), 101.4% (RSD 2.7%) and 103.2% (RSD 1.6%), respectively. Conclusion: The developed method of the HPLC-fingerprint and quantitative analysis showed good specificity, precision, reproducibility, stability and could be used for the quality control of Bailing capsules.
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