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[摘要]
目的 建立高效液相色譜-熒光檢測法測定α-生育酚的方法。方法 建立高效液相色譜-熒光檢測法,采用Merck LiChrosorb Si60(4×250 mm,5 μm)硅膠柱、熒光檢測器,以0.75%異丙醇的正己烷溶液為流動相,考察方法專屬性、線性關系、檢測限與定量限、精密度、加樣回收率、穩(wěn)定性,并與高效液相色譜-紫外檢測法進行靈敏度比較;檢測ω-3羧酸膠囊、維生素A棕櫚酸酯和維生素E中α-生育酚含量,與高效液相色譜-紫外檢測法檢測結(jié)果進行比較。結(jié)果 建立的高效液相色譜-熒光檢測法中α、β、γ和δ-生育酚分離良好,在3~30 μg/mL呈良好的線性關系(r=0.999 8);信噪比約為1:10,定量限為0.15 μg/mL;信噪比約為1:3,檢測限為0.05 μg/mL;添加ω-3羧酸、維生素A棕櫚酸酯、維生素E,加樣回收率分別為(98.7±1.4)%、(97.6±0.8)%、(99.5±2.3)%(n=9);精密度、穩(wěn)定性均符合要求;熒光檢測器較紫外檢測器靈敏度高3~5倍,且受其它主藥成分干擾??;應用兩種方法檢測的3種產(chǎn)品中α-生育酚含量相近。結(jié)論 該方法靈敏、準確、簡便,專屬性好,可用于測定多種脂溶性藥物中α-生育酚的含量。
[Key word]
[Abstract]
Objective To establish a method to determine the content of α-tocopherol in fat-soluble drugs by high performance liquid chromatography (HPLC) with fluorescence detection. Method Merck LiChrosorb Si60 silica gel column (4 mm × 250 mm, 5 μm) and fluorescence detector were adopted to establish HPLC-fluorescence detection. The mobile phase was 0.75% isopropyl alcohol in n-hexane. The specific properties, linear relations, detection limits and quantitative limits, precision, rate of recovery, and stability of the established methods were investigated, and its sensitivity was compared with that of HPLC-UV detection. The contents of α-tocopherol in Omega -3 carboxylic acid capsules, vitamin A palmitate and vitamin E were detected and compared with those of HPLC with UV detection. Results From the method established in this study, good separation of α, β, γ, and δ-tocopherol could be achieved, and the standard curve has a good linear relation in the range of 3~30 μg/mL (r= 0.999 8). The signal-to-noise ratio was 1:10, and the limit of quantification was 0.15 μg/mL; Signal-to-noise ratio was 1:3, and the detection limit was 0.05 μg/mL. After adding Omega -3 carboxylic acid, vitamin A palmitate and vitamin E, the recoveries were (98.7 + 1.4)%, (97.6 + 0.8)% and (99.5 + 2.3)%, respectively (n= 9). Precision and stability are in line with the requirements of a UV detector. The sensitivity of fluorescence detector is 3~5 times higher than that of UV detector, and is less disturbed by other main components. The contents of α-tocopherol in three products detected by two methods were similar. Conclusion This method is sensitive, accurate, simple, and good specificity, and will be used for the determination of the content of α-tocopherol in various fat-soluble drugs.
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