超高效液相色谱-串联质谱法测定果蔬中双胍三辛烷基苯磺酸盐残留量

Determination of iminoctadine tris(albesilate)residues in fruits and vegetables by ultra performance liquid chromatography-tandem mass spectrometry

建立了超高效液相色谱-串联质谱法测定水果蔬菜中双胍三辛烷基苯磺酸盐残留量。选择沃柑、橘子、橙子、苹果、西瓜、葡萄、番茄、黄瓜为样品,用25%(V/V)丙酮溶液(含1%(V/V)甲酸)提取,上清液用50%(V/V)甲醇溶液(含0.5%(V/V)甲酸)稀释后分析。以Kinetex 2.6μm Biphenyl 10 nm色谱柱(100 mm×3.0 mm)为分析柱,5 mmoL/L甲酸铵水溶液(含0.1%(V/V)甲酸)和0.1%(V/V)甲酸甲醇为流动相梯度洗脱,电喷雾离子源正离子多反应监测(MRM)模式下,以双胍辛胺的双电荷加合离子[M+2H]^(2+)m/z:178.7为母离子,与其子离子m/z:157.8,187.3,280.5组建MRM离子对进行检测,基质匹配外标法定量。结果表明,双胍三辛烷基苯磺酸盐在0.1~100.0 ng/mL范围内呈良好的线性关系,相关系数(r)均大于0.999;平均回收率在72.2%~109.5%之间,相对标准偏差为1.3%~17%;方法检出限2μg/kg,定量限4μg/kg。方法可用于果蔬中双胍三辛烷基苯磺酸盐残留量的测定。

A method was established for the determination of iminoctadine tris(albesilate)residues in fruits and vegetables by ultra performance liquid chromatography-tandem mass spectrometry.Citrus,tangerine,orange,apple,watermelon,grape,tomato and cucumber were selected as analytical samples.The samples were extracted with 25%(V/V)acetone solution(containing 1%(V/V)formic acid).The supernatant was diluted 10times with 50%(V/V)methanol solution(containing 0.5%(V/V)formic acid)and analyzed.Kinetex 2.6μm Biphenyl 10 nm column(100 mm×3.0 mm)was used as the analytical column.The mobile phase was consisted of 5 mmoL/L ammonium formate solution(containing 0.1%(V/V)formic acid)and 0.1%(V/V)formic acid methanol.The electrospray ionization source was operated in the positive ion mode under multiple reaction monitoring(MRM)mode.The double charge adduct ion[M+2H]^(2+)of guanoctine with m/z of 178.7 as the parent ion,and its daughter ions with m/z of 157.8,187.3 and 280.5 were used to form MRM ion pairs for detection.The matrix-matched external standard method was used for quantification.The results showed that there was a good linear relationship of iminoctadine tris(albesilate)in the range of 0.1-100.0 ng/mL,and the correlation coefficient(r)was greater than 0.999.The average recoveries were 72.2%-109.5%,and the relative standard deviations were 1.3%-17%.The detection limit was 2μg/kg,and the quantitation limit was 4μg/kg.The method can be used for the determination of iminoctadine tris(albesilate)residues in fruits and vegetables.