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    QuEChERS-高效液相色谱-串联质谱法测定水果中5种链格孢霉毒素

    HPLC-MS/MS Determination of 5 Alternaria Toxins in Fruits with QuEChERS

    • 摘要: 匀浆后的水果样品用1%甲酸乙腈溶液超声提取30 min,离心后,取上清液加入N-丙基乙二胺和C18净化,离心后过0.22 μm滤膜,采用高效液相色谱-串联质谱法测定滤液中5种链格孢霉毒素的含量。以Hypersil GOLD色谱柱为固定相,以不同体积比的乙腈和0.1%(体积分数,下同)甲酸溶液的混合液为流动相进行梯度洗脱,串联质谱分析中采用电喷雾离子源和多反应监测模式。5种链格孢霉毒素的质量浓度在一定范围内与其对应的峰面积呈线性关系,方法的测定下限(10S/N)为0.02~1.0 μg·kg-1。以空白样品为基体进行加标回收试验,所得回收率为93.3%~111%,测定值的相对标准偏差(n=6)为3.0%~9.7%。

       

      Abstract: After homogenate, the fruit sample was extracted ultrasonically for 30min with acetonitrile (containing 1% formic acid). After centrifugation, the supernatant was taken and then N-propyl ethylenediamin and C18 were added for purification. After centrifugation, the mixture was filtered with 0.22 μm filter membrane. HPLC-MS/MS was applied to the determination of 5 Alternaria toxins in the filtrate. Hypersil GOLD chromatographic column was used as stationary phase, and the mixture of acetonitrile and 0.1% (φ, the same below) formic acid solution mixed in different ratios was used as mobile phase in gradient elution. ESI and multi-reactions monitor mode were adopted in MS/MS. Linear relationships between values of peak area and mass concentration of the 5 Alternaria toxins were kept in definite ranges, with lower limits (10S/N) of determination in the range of 0.02-1.0 μg·kg-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 93.3%-111%, with RSDs (n=6) of determined values in the range of 3.0%-9.7%.

       

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