HPLC-MS/MS Determination of Residual Amount of 4-Chlorophenoxyaceticacid in Foodstuffs
标 签 高效液相色谱-串联质谱法 对氯苯氧乙酸 固相萃取 食品 HPLC-MS/MS 4-Chlorophenoxyacetic acid Solid Extraction Foodstuffs
提出了高效液相色谱-串联质谱法测定食品中对氯苯氧乙酸残留量的方法。食品样品经乙酸乙酯提取,过Waters Oasis MAX固相萃取小柱净化。用1.0 mL流动相溶解残渣,经ZORBOX SB-C18(50 mm×2.1 mm,3.5 μm)色谱柱分离,用乙腈-0.1%甲酸溶液(45+55)洗脱,采用电喷雾负离子模式多反应监测。对氯苯氧乙酸的质量浓度在500 μg·L-1以内与峰面积呈线性关系,检出限(3S/N)为1 μg·kg-1。取空白样品在3个标准加入水平下进行了回收和精密度试验,回收率在70.5%~99.8%之间,测定值的相对标准偏差(n=10)在4.6%~10.6%之间。
HPLC-MS/MS was applied to the determination of residual amount of 4-chlorophenoxyacetic acid in foodstuffs. The sample was extracted with ethyl acetate and purified by passing through Waters Oasis MAX solid phase extraction column. The eluate was dissolved with 1 mL of mobile phase and used for HPLC-MS/MS determination, in which ZORBAX SB-C18 column (50 mm×2.1 mm, 3.5 μm) was used as chromatographic column, and a mixture of acetonitrile and 0.1% methane acid (in the ratio of 45 to 55 by vol.) was used as mobile phase; negative electrospray ionization as well as multiple reaction monitoring mode was used in the detection. Linear relationship between values of peak area and mass concentration of 4-chlorophenoxyaceticacid was obtained in the range within 500 μg·L-1, with detection limit (3S/N) of 1 μg·kg-1. Tests for recovery and precision were made by standard addition method at 3 different concentration levels, values of recovery found were in the range of 70.5%-99.8%, and values of RSD′s (n=10) were in the range of 4.6%-10.6%.
引用该论文: FENG Jia-wang,WU Jie-shan,CAO Gui-yun,SHU Xiao-jun,REN Yong-xia,LIANG Ning. HPLC-MS/MS Determination of Residual Amount of 4-Chlorophenoxyaceticacid in Foodstuffs[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2012, 48(10): 1219～1221
冯家望,吴洁珊,曹桂云,束晓珺,任永霞,梁宁. 高效液相色谱-串联质谱法测定食品中对氯苯氧乙酸的残留量[J]. 理化检验－化学分册, 2012, 48(10): 1219～1221