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%.
出处
《分析化学》
SCIE
EI
CAS
CSCD
北大核心
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~~
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
Isotope-coded derivatization
High performance liquid chromatography-tandem mass spectrometry
Plant growth regulators