An efficient method for analyzing 2,4-Epibrassinolide in different teas was developed based on ultra-performance liquid chromatography coupled to tandem mass spectrometry (UPLC-MS/MS). Homogenized samples were extracted with acetonitrile solution, cleaned up with three sorbents including C18, strong anion exchanger (SAX) and graphitized carbon black (GCB). The compound was separated on a HSS T3 column using electrospray Ionization (ESI) mode, detected by scheduled multiple reaction monitoring (SMRM) and quantified by matrix-matched external standard curves. The compound showed good linearity between the concentration of 0.8-800βμg·L-1, with high significant correlation (R2>0.999). The limit of quantitation (LOQ, S/N=10) ranged from 0.55 to 1.46βμg·kg-1. In addition, the spiked (20, 40, 200βμg·kg-1) recoveries of tea samples were 75.5%-93.6%, and RSDs were 0.4%-7.0%. The method was accurately and sensitively applied to commercial tea samples, which fulfilled all requirement for the determination of 2,4-Epibrassinolide in tea samples.
ZHU Li
,
CHEN Hongping
,
CHAI Yunfeng
,
MA Guicen
,
HAO Zhenxia
,
WANG Chen
,
LIU Xin
,
LU Chengyin
. Determination of 2,4-Epibrassinolide in Different Teas by Ultra Performance Liquid Chromatography Coupled to Tandem Mass Spectrometry with Dispersive Solid Phase Extraction[J]. Journal of Tea Science, 2018
, 38(6)
: 589
-594
.
DOI: 10.13305/j.cnki.jts.2018.06.005
[1] Grove M D, Spencer G F, Rohwedder W K, et al.A unique plant growth promoting steroid from Brassica napus pollen[J]. Nature, 1979, 281: 216-217.
[2] 王广聚, 董服灿, 董建军. 24-表油菜素内酯的合成及应用研究[J].Pesticides, 2001, 40(6) : 12-15.
[3] 朱永兴. 茶树生长调节剂的研究与应用[J]. 中国茶叶, 1998, 20(2) : 12-13.
[4] 陆剑飞. 四种植物生长调节剂对茶叶产量与品质的影响[J]. 浙江农业学报, 2006, 18(3) : 192-194.
[5] Lee K J, Johnson V, Blakley B.The effect of exposure to a commercial 2,4-D formulation during gestation on the immune response in CD-1 mice[J]. Toxicology, 2001, 165(1) : 39-49.
[6] Erin N, Afacan B, Ersoy Y.Gibberellic acid, a plant growth regulator, increases mast cell recruitment and alters Substance P levels[J]. Toxicology, 2008, 254(1/2) : 75-81.
[7] Tuluce Y, Celik I.Effects of indole-3-acetic acid and kinetin on the adenosine deaminase activity in various tissues of rats[J]. Asian Journal of Chemistry, 2006, 18(1) : 528-532.
[8] Cao L D, Yang J, Li X H, et al.Determination of brassinolide analogs by high-performance liquid chromatography with evaporative light scattering detection[J]. Analytical Letters, 2015, 48(4): 575-585.
[9] Lv T, Zhao X E, Zhu S Y.et al.Development of an efficient hplc fluorescence detection method for brassinolide by ultrasonic-assisted dispersive liquid-liquid microextraction coupled with derivatization[J]. Chromatographia, 2014, 77(23/24): 1653-1660.
[10] Oklestkova J, Tarkowska D, Eyer L, et al.Immunoaffinity chromatography combined with tandem mass spectrometry: A new tool for the selective capture and analysis of brassinosteroid plant hormones[J]. Talanta, 2017, 170: 432-440.
[11] Ding J, Mao L J, Wang S T, et al.Determination of endogenous brassinosteroids in plant tissues using solid-phase extraction with double layered cartridge followed by high-performance liquid chromatography- tandem mass spectrometry[J]. Phytochemical Analysis, 2013, 24(4): 386-394.
[12] Huo F F, Wang X, Han Y H, et al.A new derivatization approach for the rapid and sensitive analysis of brassinosteroids by using ultra high performance liquid chromatography-electrospray ionization triple quadrupole mass spectrometry[J]. Talanta, 2012, 99: 420-425.
[13] Jiao W T, Xiao Y, Qian X S, et al.Optimized combination of dilution and refined QuEChERS to overcome matrix effects of six types of tea for determination eight neonicotinoid insecticides by ultra performance liquid chromatography- electrospray tandem mass spectrometry[J]. Food Chemistry, 2016, 210: 26-34.
[14] Rahman M M, Abd El-Aty A M, Choi J H, et al. Consequences of the matrix effect on recovery of dinotefuran and its metabolites in green tea during tandem mass spectrometry analysis[J]. Food Chemistry, 2015, 168: 445-453.
[15] Zhang K, Wong J W, Yang P, et al.Protocol for an electrospray ionization tandem mass spectral product ion library: development and application for identification of 240 pesticides in foods[J]. Analytical Chemistry, 2012, 84(13): 5677-5684.
[16] 诸力, 王晨, 陈红平, 等. 超高效液相色谱-串联质谱法同时测定茶叶中11种植物生长调节剂及吡虫啉、啶虫脒的残留[J]. 分析化学, 2017, 45(4): 529-536.
[17] 虞冰, 刘莉, 汪志威, 等. QuEChERS-超高效液相色谱-串联质谱法快速测定草莓中2,4-表芸苔素内酯残留量[J]. 浙江农业科学, 2017, 58(9): 1538-1540, 1545.
[18] Kittlaus S, Schimanke J, Kempe G, et al.Assessment of sample cleanup and matrix effects in the pesticide residue analysis of foods using postcolumn infusion in liquid chromatography-tandem mass spectrometry[J]. Journal of Chromatography A, 2011, 1218(46): 8399-8410.
浙公网安备 33019902000101号 
