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出 处:《分析试验室》2011年第1期87-89,共3页Chinese Journal of Analysis Laboratory
摘 要:建立了同时检测丁丙诺啡和纳洛酮的超高效液相色谱的分析方法。分析柱为Waters Acquity BEH C18超高效液相色谱柱,紫外检测波长为280nm,流动相为甲醇-甲酸(0.2%)水,梯度洗脱,两种分析物在3min内即可达到良好分离。纳洛酮和丁丙诺啡的线性范围分别为1~25μg/mL,2~50μg/mL,线性相关系数分别为0.9992,0.9995。检出限为0.2μg/mL。考察了甲醇和乙腈两种流动相体系对样品的分离效果,发现甲醇流动相体系的响应高于乙腈流动相体系。在优化条件下,对丁丙诺啡舌下含片以及加标后样品进行测定,且对其方法学进行考察,加标平均回收率在91.3%~100.1%之间,RSD小于5%。A simultaneous method was established for the separation and determination of buprenorphine and naloxone in buprenorphine sublingual tablets by ultra-high performance liquid chromatography.The samples were separated on a Waters Acquity BEH C18 column with gradient elution using methanol and water(containing 0.2% formic),the two compounds were effectively separated in 3 min,and the detection was performed with an UV dector at the wavelength of 280 nm.The linear ranges of the compounds were from 1 to 25 μg/mL for naloxone and 2 to 50 μg/mL for buprenorphine,the correlation coefficients were 0.9992 and 0.9995,respectively,and the limits of detection(LOD) of the method for the two compounds were 0.2 μg/mL.A comparative study of two mobile phase systems methanol and acetonitrile were performed,and the response of methanol is higher than that for acetonitrile.Under optimum conditions,the actual buprenorphine sublingual tablets and spiked samples were determined.The average recoveries were 91.3%~100.1%,and RSD less than 5%.
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