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

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2.0000 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-C_(18)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(M R M)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1.0~200.0μg·L^(-1)内与其峰面积呈线性关系,检出限(3S/N)为0.01~0.04μg·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%。

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.2.0000 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 ethylencdiamine(1.00 g)and anhydrous magnesium sulfate(0.20 g)by dispersive solid phase extraction.The purified solution was then separated on ZORBAX XDB-C_(18)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 1.0-200.0μg·L^(-1),with detection limits(3 S/N)in the range of 0.01-0.04μg·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%.