方法验证二氧化硅分散固相萃取-紫外可见分光光度法测定中草药中别嘌呤醇

E. R. Amanda, Anisa Suci Rosmawati, Lilik Nurfadlilah, G. Buono, Yani Ambari
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引用次数: 1

摘要

成功建立了二氧化硅分散固相萃取-紫外-可见分光光度计联合提取草药中别嘌呤醇的简便制样方法。二氧化硅作为固体吸附剂。提取过程是将二氧化硅插入并分散在含有别嘌呤醇的30 mL样品溶液中,然后用热板搅拌器搅拌。在提取过程的最后,二氧化硅被收集起来,用乙醇通过涡流解吸。用紫外-可见分光光度计对解吸液进行分析,最大波长为250 nm。对样品质量、萃取时间、解吸时间、pH等关键参数进行了优化。结果表明,最佳提取条件为二氧化硅质量。0.8克;提取时间,45分钟;解吸时间,2分钟;样品溶液的pH值为ph7。将最佳提取条件应用于标准曲线的绘制,并对中药样品中的别嘌呤醇进行了分析。方法验证结果得到相关系数(R2)为0.9961;检出限:0.6871 ppm;定量限为2.2902 ppm,加样回收率(% R)为96.42 ~ 110.25%,变异系数(% CV)为0.0361 ~ 0.1322%。对3个实际样品的应用方法表明,别嘌呤醇的浓度分别为56.0221 ppm、54.8706 ppm和63.6719 ppm。用峰值法分析实际样品的% R值在49.52 ~ 89.74%之间。
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Method Validation of Silica Dispersive Solid Phase Extraction Combined with Spectrophotometer UV-Vis for the Determination of Allopurinol in Herbal Medicine
A facile sample preparation method based on silica dispersive solid-phase extraction combination with spectrophotometer UV-Vis for the extraction of allopurinol in herbal medicine was successfully developed. Silica was used as a solid sorbent. The extraction process was carried out by inserting and dispersing silicas in a 30 mL sample solution that contained allopurinol, then stirred using a hot plate stirrer. At the end of the extraction process, silicas were collected and desorbed using ethanol by utilizing a vortex. The desorption solution was analyzed by spectrophotometer UV-Vis at a maximum wavelength of 250 nm. Several essential parameters such as silica mass, extraction time, desorption time, and pH of sample solution were optimized. The results showed that the optimum extraction condition was achieved: silica mass. 0.8 grams; extraction time, 45 minutes; desorption time, 2 minutes; and pH of sample solution, pH 7. The optimum extraction condition was then applied for the standard curve and analyzed of allopurinol in herbal medicine samples. The results of the method validation method were obtained the correlation coefficient (R2), 0.9961; the detection limit, 0.6871 ppm; the quantitation limit, 2.2902 ppm, the percent of recovery (% R) in the range of 96.42-110.25%, percent coefficient of variation (% CV) in the range of 0.0361- 0.1322%. The application method in 3 real samples showed that the concentrations of allopurinol were 56.0221 ppm, 54.8706 ppm, and 63.6719 ppm, respectively. The values of % R in the analysis of real samples by using the spiking method were obtained in the range of 49.52-89.74%.
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