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    高效液相色谱-串联质谱法测定葡萄酒中4种有机磷类除草剂残留量

    Determination of 4 Organophosphorous Herbicides Residues in Grape Wine by HPLC-MS/MS

    • 摘要: 提出了同时测定葡萄酒中莎稗磷、甲基胺草磷、抑草磷和哌草磷4种有机磷类除草剂残留量的高效液相色谱-串联质谱法。样品2.000 0 g加入12 mL的乙酸乙酯和1.00 g氯化钠,涡旋混匀30 s,超声提取10 min,提取液经1.00 g PSA、0.20 g无水硫酸镁分散固相萃取净化。采用ZORBAX XDB-C18色谱柱进行分离,以体积比15∶85的0.1%(体积分数)甲酸溶液和甲醇的混合液为流动相进行等度洗脱。以电喷雾离子源正离子(ESI+)和多反应监测(MRM)模式进行质谱分析,外标法定量。4种有机磷类除草剂的质量浓度在1.0~200.0 μg·L-1内与其峰面积呈线性关系,检出限(3S/N)为0.01~0.04 μg·kg-1。采用标准加入法在3个浓度水平上进行回收试验,回收率为69.3%~99.2%,测定值的相对标准偏差(n=5)为2.3%~8.1%。

       

      Abstract: HPLC-MS/MS was proposed for the determination of the residual anount of 4 organophosphorus herbicides, including paspalum, methamphoron, imphoron, and piperon in grape wine. 2.000 0 g of samples were mixed with 12 mL of ethyl acetate and 1.00 g of sodium chloride by vertical oscillation for 30 s, and the solution was extracted ultrasonically for 10 min. The extract was purified with N-propyl ethylenediamine (1.00 g) and anhydrous magnesium sulfate (0.20 g) by dispersive solid phase extraction. The purified solution was then separated on ZORBAX XDB-C18 column as stationary phase and the mixture of 0.1% (φ) formic acid solution and methanol with the volume ratio of 15 to 85 was used as mobile phase in isocratic elution. ESI+ and MRM were adopted in MS analysis, and external standard method was used for quantification. Linearity relationships between values of peak area and mass concentration of 4 organophosphorus herbicides were kept in the same range of 1.0-200.0 μg·L-1, with detection limits (3S/N) in the range of 0.01-0.04 μg·kg-1. Test for recovery was made by standard addition at 3 different concentration levels, giving results in the range of 69.3%-99.2%, with RSDs of determined values (n=5) ranged from 2.3% to 8.1%.

       

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