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首次建立了反相液相色谱仪同时测定乳粉中8种生育酚和生育三烯酚(α-、β-、γ-及δ-生育酚,α-、β-、γ-及δ-生育三烯酚)的检测方法。具体条件为:流动相为水-甲醇[体积比,(0~14.0)min:85%~95%;(14.01~20.0)min:95%~85%],流速:1.0 m L/min;柱温:30℃;激发波长Ex=290 nm,发射波长Em=330 nm;进样体积10μL,外标法定量。在14 min内同时分离出8种V_E异构体,8种目标物的线性范围分别为(0.100~40.0)μg/m L、(0.200~40.0)μg/m L、(0.500~40.0)μg/m L,8种目标物在各自的质量范围内线性关系良好(r>0.9999),8种化合物的检出限为(0.010~0.20)μg/m L,定量限为(0.040~0.67)μg/m L,在3个添加水平下的平均加标回收率为84.9%~96.2%、87.2%~92.1%、80.7%~91.2%,相对标准偏差(RSD)为0.67%~3.3%(n=3)。该方法准确、高效、结果可靠,适用于乳粉中8种生育酚和生育三烯酚的同时测定。该方法通过高效液相色谱法完成了100多种市售乳粉中V_E的测定,并与营养标签进行比较。
For the first time, a reversed-phase liquid chromatograph was developed for the simultaneous determination of 8 tocopherols and tocotrienols (α-, β-, γ- and δ-tocopherols, α-, β-, γ- and δ- Triene) test method. The specific conditions are as follows: the mobile phase is water-methanol [volume ratio (0-14.0) min: 85-95%; (14.01-20.0) min: 95-85% Temperature: 30 ℃; excitation wavelength Ex = 290 nm, emission wavelength Em = 330 nm; injection volume 10 μL, external standard method. The linear ranges of the eight target compounds were (0.100 ~ 40.0) μg / mL, (0.200 ~ 40.0) μg / mL and (0.500 ~ 40.0) μg / The linear range was 0.9999. The detection limits of the eight compounds ranged from (0.010-0.20) μg / m L and the limits of quantitation (0.040-0.67) μg / m L, the average recoveries were 84.9% ~ 96.2%, 87.2% ~ 92.1%, 80.7% ~ 91.2% and the relative standard deviations (RSDs) were 0.67% ~ 3.3% ). The method is accurate, efficient and reliable. It is suitable for the simultaneous determination of eight kinds of tocopherols and tocotrienols in milk powder. The method was used to determine the V_E of more than 100 kinds of commercial milk powder by HPLC, and compared with the nutrition label.