Li Bo, Deng Xiaojun, Guo Dehua, Jin Shuping
Shanghai Entry-Exit Inspection and Quarantine Bureau, Shanghai 200135, China.
Se Pu. 2007 Jul;25(4):486-90.
A method for the determination of glyphosate (PMG) and aminomethylphosphonic acid (AMPA) residues in plant products, such as rice, wheat, vegetables, fruits and tea, pig and chicken muscles, aquatic products, chestnut, honey, etc., was developed using high performance liquid chromatography coupled to tandem mass spectrometry (HPLC-MS/MS). In this method, PMG and AMPA were extracted with water from samples, defatted using an extraction step with dichloromethane, and purified using a cation-exchange (CAX) solid phase extraction cartridge. Then, these were derived using fluorenylmethylchloroformate (FMOC-Cl) in borate buffer for subsequent HPLC-MS/MS analysis. Isotope-labeled PMG 1, 2(13)- C(15) N was used as the internal standard for the quantitative analysis of two residues. For all samples, the recoveries ranged from 80.0% to 104% and the relative standard deviations (RSDs) ranged from 6.7% to 18.2%. The limit of quantification (LOQ) was determined to be 0.05 mg/kg with a linear range of 0.20-10 microg/L. It is demonstrated that this method is reliable and sensitive for the analysis of PMG and APMA with low concentrations in foods.
建立了一种利用高效液相色谱-串联质谱法(HPLC-MS/MS)测定植物产品(如大米、小麦、蔬菜、水果和茶叶)、猪鸡肉、水产品、栗子、蜂蜜等中草甘膦(PMG)和氨甲基膦酸(AMPA)残留量的方法。该方法中,PMG和AMPA用水从样品中提取,通过二氯甲烷萃取步骤脱脂,并用阳离子交换(CAX)固相萃取柱净化。然后,在硼酸盐缓冲液中用氯甲酸芴甲酯(FMOC-Cl)衍生化,用于后续的HPLC-MS/MS分析。同位素标记的PMG 1, 2(13)-C(15)N用作两种残留量定量分析的内标。所有样品的回收率在80.0%至104%之间,相对标准偏差(RSD)在6.7%至18.2%之间。定量限(LOQ)确定为0.05 mg/kg,线性范围为0.20 - 10 μg/L。结果表明,该方法对于分析食品中低浓度的PMG和APMA是可靠且灵敏的。