高级检索

    超高效液相色谱-串联质谱法测定茶叶中百草枯

    UHPLC-MS/MS Determination of Paraquat in Tea

    • 摘要: 采用超高效液相色谱-串联质谱法测定茶叶中百草枯的含量。均质茶叶样品(2±0.02) g用硫酸(7+13)溶液提取,提取液5 mL通过固相萃取柱净化,再用5 mol·L-1氯化铵溶液15 mL洗脱。在洗脱液中加入12 mol·L-1氢氧化钠溶液12 mL,10 g·L-1铁氰化钾溶液1 mL后,用二氯甲烷提取两次(每次20 mL),合并二氯甲烷层,并将其蒸干。用乙腈(1+9)溶液2 mL溶解残渣,并过0.22 μm有机系滤膜。以Waters BEH UPLC C18色谱柱为分离柱,以不同体积比的乙腈和乙腈(5+95)溶液的混合液为流动相进行梯度洗脱,采用电喷雾正离子源和多反应监测模式检测。百草枯的质量浓度在0.001~0.1 mg·L-1内与其对应的峰面积呈线性关系,检出限(3S/N)为0.5 μg·L-1。在10,100 μg·kg-1等2个浓度水平进行加标回收试验,回收率依次为71.0%,89.2%,测定总量的相对标准偏差(n=6)依次为11%,1.1%。

       

      Abstract: UHPLC-MS/MS was applied to the determination of paraquat in tea. (2±0.02) g of homogenized sample of tea was extracted with H2SO4 (7+13) solution. The extract (5 mL) was purified by passing through SPE column, and then 15 mL of 5 mol·L-1 NH4Cl solution was used for elution. 12 mL of 12 mol·L-1 NaOH solution and 1 mL of 10 g·L-1 potassium ferricyanide solution were added in the eluate. The solution was extracted twice with dichloromethane (20 mL each). The combined dichloromethane layer was evaporated to dryness. The residue was taken up with 2 mL of acetonitrile (1+9) solution, and then the solution was filtered on 0.22 μm organic filtering membrane. Waters BEH UPLC C18 chromatographic column was used as stationary phase, and the mixture of acetonitrile and acetonitrile (5+95) 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 relationship between values of peak area and mass concentration of paraquat was kept in the range of 0.001-0.1 mg·L-1, with detection limit (3S/N) of 0.5 μg·L-1. Tests for recovery were made by standard addition method at the concentration levels of 10, 100 μg·kg-1, giving values of recovery of 71.0%, 89.2% and RSD's (n=6) of 11%, 1.1%, respectively.

       

    /

    返回文章
    返回