摘要
该文建立了一种基于QuEChERS前处理的超高效液相色谱-质谱法(UPLC-MS/MS),该方法能快速、准确地测定葡萄中10种植物生长调节剂(PGRs)的残留量。样品用含1%甲酸的乙腈溶液提取,经QuEChERS净化处理,以Thermo Accucore C18色谱柱(2.1 mm×100 mm,1.7μm)为固定相,流动相A为含0.1%甲酸和2.5 mmol/L甲酸铵的水溶液,流动相B为含0.1%甲酸和2.5 mmol/L甲酸铵的甲醇溶液,梯度洗脱;质谱分析以电喷雾离子源(ESI源)电离喷雾,多反应监测(MRM)模式,外标法定量。10种PGRs质量浓度在0~200 ng/mL范围内线性良好,相关系数(R^(2))≥0.9980,在10、50、100μg/kg 3个浓度水平下,加标回收率为71.5%~101.8%,相对标准偏差(RSD)为1.8%~8.8%,方法检出限为1.0~2.5μg/kg,定量限为3.0~8.0μg/kg。该方法操作简便、分析时间短,可快速、高效地测定葡萄中10种PGRs残留量,对实现葡萄种植过程管控、日常监管、质量保障具有重要意义。
This paper established a method of ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)based on QuEChERS pretreatment,this method could quickly and accurately determine the residual levels of 10 plant growth regulators(PGRs)in grapes.Samples were extracted with acetonitrile solution containing 1%formic acid,purified by QuEChERS,a Thermo Accucore C18 column(2.1 mm×100 mm,1.7μm)was used as the stationary phase,and gradient elution was performed with mobile phase A:0.1%formic acid and 2.5 mmol/L ammonium formate aqueous solution and mobile phase B:0.1%formic acid and 2.5 mmol/L ammonium formate methanol solution.Mass spectrometry analysis was carried out using electric spray ion source(ESI source),ionization spray and multiple reaction monitoring(MRM)mode,and the external standard method was used for quantitative analysis.The mass concentration of 10 PGRs showed good linearity in the range of 0~200 ng/mL,with correlation coefficients(R^(2))≥0.9980.At 3 concentration levels of 10,50,100μg/kg,the spiked recovery rate ranged from 71.5%~101.8%,and the relative standard deviation(RSD)was 1.8%~8.8%.The detection limit of the method was 1.0~2.5μg/kg,and the quantitation limit was 3.0~8.0μg/kg.The method is simple to operate,has a short analysis time,and can quickly and efficiently analyze 10 PGRs residues contents in grapes.It is of great significance to achieve process control,daily supervision,and quality assurance in grape cultivation.
作者
黄文
卢军
王蓓蓓
缑慧君
丁伟
黄微
马玉凤
彭露湫
王佳
马骞
HUANG Wen;LU Jun;WANG Beibei;GOU Huijun;DING Wei;HUANG Wei;MA Yufeng;PENG Luqiu;WANG Jia;MA Qian(Hanzhong Food and Drug Supervision Inspection and Testing Center,Hanzhong 723000,China)
出处
《食品与发酵科技》
2025年第4期140-144,共5页
Food and Fermentation Science & Technology
关键词
超高效液相色谱-质谱
QUECHERS
植物生长调节剂
葡萄
ultra performance liquid chromatography-tandem mass spectrometry
QuEChERS
plant growth regulators
grapes
