首页> 中文期刊> 《分析化学》 >同位素编码衍生-高效液相色谱串联质谱法测定果蔬样品中的羧酸类植物生长调节剂

同位素编码衍生-高效液相色谱串联质谱法测定果蔬样品中的羧酸类植物生长调节剂

         

摘要

A method for determination of 6 plant growth regulators by high performance liquid chromatography-tandem mass spectrometry ( HPLC-MS/MS ) coupled with isotope-coded derivatization was developed. d0-10-Methyl-acridone-2-sulfonyl piperazine ( d0-MASPz, light form) and d3-10-methyl-acridone-2-sulfonyl piperazine ( d3-MASPz, heavy form ) were prepared as isotope-coded derivatization reagents for carboxyl compound. The carboxyl plant growth regulator standards and real samples were derivatized by d0-MASPz and d3-MASPz, respectively. The obtained solutions were mixed at a certain ratio, and then injected for HPLC-MS/MS analysis. The light and heavy derivatives were monitored with transitions of [M+H]+m/z 208. 2 and [M+H]+ m/z 211. 2,respectively. With heavy derivative as internal standard for corresponding light derivative, the global isotope internal standard quantification for 6 plant growth regulators was achieved. The results indicated that the proposed isotope-coded derivatization method could provide relative quantitative data with adequate linearity in a 10-fold dynamic range ( R=0 . 9991 ) . The detection and quantitation limits were 0. 19-0. 34 μmol/L and 0. 53-0. 96 μmol/L, respectively. The relative standard deviations were ≤3 . 8%, and the accuracies ranged from 97 . 5% to 103 . 8%.%以d0/d3-10-甲基吖啶酮-2-磺酰哌嗪( d0/d3-MASPz)为同位素编码衍生试剂,建立了高效液相色谱串联质谱( HPLC-MS/MS)快速测定果蔬中6种羧酸类植物生长调节剂的分析方法。分别以d0-MASPz(轻型)和d3-MASPz(重型)为衍生样品和对照品,混合后进行HPLC-MS/MS分析。轻型和重型衍生物分别以[ M+H]+m/z 208.2和[M+H]+ m/z 211.2作为多级反应监测离子对,以重型衍生物作为相应轻型衍生物的内标物,建立定量分析方法。结果表明,在6.5 min内可实现6种分析物的完全分离,轻/重衍生物保留时间差异小于0.026 min,6种分析物的轻/重信号强度比在10倍动态范围内线性关系良好,相关系数r>0.9991,检测限和定量限分别为0.19~0.34μmol/L和0.53~0.96μmol/L,相对标准偏差小于3.8%,标准加入的回收率为95.3%~105.5%之间。

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