摘要
目的建立测定金水宝胶囊中腺苷及腺嘌呤含量的高压液相色谱方法。方法采用0.5%磷酸超声提取制备金水宝胶囊样品溶液,色谱柱为Venusil-XBP-C18(250 mm×4.6 mm,5μm);流动相采用[0.01 mol.L-1 NaH2PO4∶0.01 mol.L-1 Na2HPO4(1∶2.2,V/V)]∶甲醇(17∶3,V/V),流速0.6 mL.min-1,进样量10μL,柱温25℃,检测波长260 nm,运行时间18 min。运行时用流动相∶甲醇(85∶15,V/V)梯度洗脱。结果腺苷及腺嘌呤分别在0.62～157.07 mg.L-1和0.23～58.29 mg.L-1内线性关系良好;两者的平均回收率分别为(97.40±4.28)%和(99.10±5.03)%;3种批号的金水宝胶囊样品中腺苷的含量分别为(0.324±0.017)%、(0.318±0.025)%和(0.331±0.019)%;腺嘌呤的含量分别为(0.089±0.009)%、(0.086±0.012)%和(0.093±0.007)%。结论高效液相色谱法测定金水宝胶囊中腺苷及腺嘌呤的含量操作简便、结果准确可靠、灵敏度高、重复性好,能作为有效控制金水宝胶囊质量的测定方法之一。
AIM To establish a HPLC method for the determination of adenosine and adenine in Jinshuibao capsules. METHODS The contents in Jinshuibao capsules were extracted with 0.5% phosphoric acid by ultrasound-assisted method. The chromatographic separation was performed on Venusil-XBP-C^8 （250 mm ~ 4.6 ram, 5μm） column with a mobile phase of [0.01 mol.L-1NaH2PO4 ： 0.01 mol.L-1Na2HPO4 （1 ： 2.2, V/V）] ： methanol （17 ： 3, V/V） at a flow rate of 0.6 mL.min-1. Injection volume was 10 μL. The detection wavelength was 260 nm and the column temperature was 25℃ Running time was 18 min. Gradient elution was performed with mobile phase ： methanol （85 ： 15, V/V）. RESULTS The linear concentration ranges for adenosine and adenine were 0.62 - 157.07 mg.L-1 and 0.23 - 58.29mg.L-1. The average recovery of adenosine and adenine were （97.40 ± 4.28） % and （99.10 ± 5.03） %, respectively. The contents of adenosine in three batches were （0.324± 0.017） %, （0.318 ± 0.025） % and （0.331 ± 0.019） %, and the contents of adenine were （0.089 ± 0.009） %, （0.086 ± 0.012） % and （0.093 ± 0.007） %, respectively. CONCLUSION This method is simple,rapid, accurate and reproducible, and is suitable for quantitative analysis of Jinshuibao capsules.
出处
《中国新药与临床杂志》
CAS
CSCD
北大核心
2011年第10期786-788,共3页
Chinese Journal of New Drugs and Clinical Remedies
关键词
色谱法
高压液相
腺苷
腺嘌呤
金水宝胶囊
chromatography, high pressure liquid
adenosine
adenine
Jinshuibao capsules
