超高效合相色谱法测定紫杉醇原料药的含量  

Determination of Content of Paclitaxel using Ultra Performance Convergence Chromatography

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作  者:齐宁利[1] 龚霄[1] 陈松[1,2] 李普旺[1] 

机构地区:[1]中国热带农业科学院农产品加工研究所,湛江524001 [2]广东海洋大学食品科技学院,湛江524088

出  处:《现代科学仪器》2014年第5期129-132,共4页Modern Scientific Instruments

基  金:海南省自然科学基金资助(No.512106)

摘  要:目的:建立快速、准确、灵敏的测定紫杉醇原料药的方法。方法:采用沃特世ACQUITY超高效合相色谱系统(UPC2)。采用ACQUITY UPC2 BEH 2-EP柱(3.0mm×100mm,1.7mm);以二氧化碳(A)-甲醇(B)二元梯度洗脱,0-0.2min(92:8,V:V),0.2-2.5min(92:8-82:18,V:V),2.5-4.0min(82:18,V:V);流速2.2m L/min;柱温50℃;备压2200 psi;进样体积2.0m L。结果:此条件下紫杉醇分离良好,在0.6-196mg/m L浓度范围内线性关系良好,回归方程为:Y=94.74X+404.67(r=0.9999),平均回收率(n=9)为99.57%,相对标准偏差为0.71%。结论:UPC2法检测快速、准确、灵敏度高、重复性好,为紫杉醇原料药的质量控制提供了一种快速准确的方法。Objective: A rapid, accurate and sensitive method is established to determine the content of paclitaxel in pharmaceutical ingredient. Method: Waters ACQUITY UPC2 was used.ACQUITY UPC2 BEH 2-EP (3.0mm× 100mm,1.7 mm) column was used with a mobile phase of CO2 and methanol, using the mobile phase of mixture of supercritical CO2 and methanol with a linear gradient elution:0-0.2 min (92:8,V:V),0.2-2.5 min (92:8-82:18,V:V),2.5-4.0 min (82:18, V:V);a flow rate was 2.2mL/min;column temperature was 50℃ ;black pressure was 2200 psi and injection volume was 2.0 mL. Result:The result showed that the paclitaxel had a good linear relationship when its concentration ranged from 0.6 and 196mg/mL,The regression equation was Y=94.74X+404.67 (r=0.9999).The average recovery of paclitaxel was 99.57% with the a relative standard deviations (RSD) of 0.71%.Conclusion:UPC2 method is rapid, accurate and sensitive with a good repeatability, and could use for quality control of paclitaxel.

关 键 词:UPC2 紫杉醇 含量测定 

分 类 号:TH833[机械工程—仪器科学与技术]

 

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