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  

Determination of Plant Growth Regulators in Vegetable by High Performance Liquid Chromatography-Tandem Mass Spectrometry Coupled with Isotope-coded Derivatization

作　　者：蔡轶平 孙志伟[1] 王小艳[2] 索有瑞[2] 尤进茂[1,2] 

机构地区：[1]曲阜师范大学,山东省生命有机分析重点实验室,曲阜273165 [2]中国科学院西北高原生物研究所,西宁810001

出　　处：《分析化学》2015年第3期419-423,共5页Chinese Journal of Analytical Chemistry

基　　金：国家自然科学基金(Nos.21305076,31300292);山东省自然科学基金(No.ZR2012BQ022)资助~~

摘　　要：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。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%.

关 键 词：同位素编码衍生 高效液相色谱串联质谱 植物生长调节剂 

分 类 号：TS255.7[轻工技术与工程—农产品加工及贮藏工程] O657.63[轻工技术与工程—食品科学与工程]