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目的:建立多烯酸乙酯软胶囊中4种生育酚的HPLC含量测定方法,同时对不同厂家产品中4种生育酚(α、β、γ、δ-生育酚)的含量进行比较。方法:采用色谱柱为MERCK Lichro CART 250-4硅胶柱(250 mm×4.6 mm,5μm),流动相为正己烷-异丙醚(80∶20),流速1.0 m L·min-1,柱温25℃,荧光检测器激发波长298 nm,发射波长325 nm。结果:4种生育酚的质量浓度均在40~1 000 ng·m L-1范围内线性关系良好(r>0.999);检出限分别为7.0、6.0、6.2、6.2 ng·m L-1;加样平均回收率为90.1%~99.7%。国内不同厂家的α-生育酚的含量范围为1.92~32.95μg·g-1,γ-生育酚范围为1.23~21.22μg·g-1,δ-生育酚范围为0.83~13.05μg·g-1,β-生育酚均未检出,国外同类品种中α-生育酚的含量约为1 800μg·g-1。结论:本文建立的生育酚的高效液相色谱-荧光检测法具有较高的灵敏度、精密度和准确性,可作为有效控制ω-3多不饱和脂肪酸乙酯类药物的产品质量的检测方法。
OBJECTIVE: To establish a HPLC method for the determination of four kinds of tocopherols in ethyl polyunsaturated soft capsules. The contents of four kinds of tocopherols (α, β, γ, δ-tocopherol) from different manufacturers were also compared. METHODS: The column was a MERCK Lichro CART 250-4 silica gel column (250 mm × 4.6 mm, 5 μm) with a mobile phase of n-hexane-isopropyl ether (80:20) at a flow rate of 1.0 m L · min- 25 ℃, fluorescence detector excitation wavelength 298 nm, emission wavelength 325 nm. Results: The four kinds of tocopherols had a good linearity (r> 0.999) in the range of 40-1 000 ng · m L-1 with detection limits of 7.0, 6.0, 6.2 and 6.2 ng · m L-1, respectively The average recovery rate was 90.1% ~ 99.7%. The content of α-tocopherol in different domestic manufacturers ranged from 1.92 to 32.95 μg · g-1, the range of γ-tocopherol ranged from 1.23 to 21.22 μg · g-1, the range of δ-tocopherol ranged from 0.83 to 13.05 μg · g-1 , β-tocopherol were not detected, foreign similar species α-tocopherol content of about 1 800 μg · g-1. Conclusion: The high performance liquid chromatography with fluorescence detection method of tocopherols established in this paper has high sensitivity, precision and accuracy and can be used as a detection method to effectively control the quality of omega-3 polyunsaturated fatty acid ethyl esters.