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    液相色谱-四极杆-静电轨道阱高分辨质谱法测定保健食品中11种磷酸二酯酶抑制剂

    Determination of 11 Phosphodiesterase Inhibitors in Health Food by LC-Quadrupole-Orbitrap High Resolution MS

    • 摘要: 保健食品样品用50%(体积分数)甲醇溶液超声提取15 min,提取液用水定容至50.0 mL,离心,取上清液,经0.22 μm微孔滤膜过滤,采用液相色谱-四极杆-静电轨道阱高分辨质谱法测定滤液中11种磷酸二酯酶抑制剂的含量。以Waters HSS T3色谱柱为固定相,以不同体积比的0.1%(体积分数)甲酸溶液和乙腈的混合液为流动相进行梯度洗脱,质谱分析中采用电喷雾离子源正离子模式和全扫描模式。11种磷酸二酯酶抑制剂的质量浓度均在2~100 μg·L-1内与其对应的峰面积呈线性关系,测定下限(10S/N)为0.02~0.5 μg·L-1。以空白样品为基体进行加标回收试验,所得回收率为75.7%~98.9%,测定值的相对标准偏差(n=6)为5.9%~14%。

       

      Abstract: The health food sample was extracted ultrasonically for 15 min with 50% (φ) methanol solution, and then the extract was diluted to 50.0 mL with water. After centrifugation, the supernatant was taken and filtered with 0.22 μm millipore filter. LC-quadrupole-orbitrap high resolution MS was applied to the determination of 11 phosphodiesterase inhibitors in the filtrate. Waters HSS T3 chromatographic column was used as stationary phase, and the mixture of 0.1% (φ) formic acid solution and acetonitrile mixed in different ratios was used as mobile phase in gradient elution. ESI+ and the full scanning mode were adopted in MS. Linear relationships between values of peak area and mass concentration of the 11 phosphodiesterase inhibitors were kept in the same range of 2-100 μg·L-1, with lower limits of determination (10S/N) in the range of 0.02-0.5 μg·L-1. On the base of blank sample, test for recovery was made by standard addition method; values of recovery found were in the range of 75.7%-98.9%, with RSDs (n=6) of determined values in the range of 5.9%-14%.

       

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