高效液相色谱-串联质谱法测定水果中多果定残留量

HPLC-MS/MS Determination of Residual Amount of Dodine in Fruits

提出了水果中多果定残留量的高效液相色谱串联质谱分析方法。样品经甲醇振荡提取3～5 min,离心分离取上清液蒸发至干。用流动相溶解残渣,经BEH C_(18)色谱柱(2.1mm×100)mm,1.7μm)分离,用乙腈与5mmol·L^(-1)乙酸铵溶液按体积比80比20混合作为流动相进行淋洗,采用正离子模式多反应监测。定性离子对为m/z 185.9,56.7,定量离子为m/z 56.7。多果定的质量浓度与其峰面积在5.0～500.0μg·L^(-1)范围内呈线性关系,测定下限(10S/N)为0.04mg·kg^(-1)。以水果样品为基体,加入3种不同浓度的多果安标准溶液做回收试验,测得回收率在80.0%～104.6%之间,相对标准偏差在4.3%～14%之间。

HPLC MS/MS was applied to the determination of residual amount of dodine in fruits. The sample was extracted with methanol by shaking for 3- 5 min. After centrifugation, the supernatant obtained was evaporated to dryness. The residue was dissolved with the mobile phase and used for HPLC-MS/MS determination, in which BEH ClS column （2. 1 mm× 100 mm, 1. 7 μm） was used as chromatographic column, and mixture of acetonitrile and 5 mmol . L-1; ammonium acetate （80＋20） was used as mobile phase; positive electrospray ionization as well as multiple reaction monitoring mode was used in the MS detection. Ion pair used for qualitative analysis was： m/z 185.9,56.7, and ion use for quantitative analysis was m/z 56. 7. Linear relationship between values of peak area and mass concentration of dodine was obtained in the range of 5.0-500. 0 μg . L 1, with lower limit of determination （10S/N） of 0.04 mg. kg-1. Tests for recovery and precision were made by addition of standard solution of dodine at 3 concentration levels to fruit samples which were then analyzed by the proposed method. Values of recovery and RSD＇s （n=10） obtained were in the ranges of 80. 0% to 104. 6% and 4. 3% to 14% respectively.