高效液相色谱-三重四极杆质谱法同时测定番茄中水杨酸和赤霉酸

建立番茄中植物激素——水杨酸和赤霉酸的高效液相色谱-三重四极杆质谱检测方法。样品经乙酸-乙腈提取,采用C_(18)固相萃取柱净化,C_(18)色谱柱分离,0.5%甲酸-甲醇溶液作为流动相进行梯度洗脱,质谱采用电喷雾负离子模式电离,多反应监测模式定性,基质标准曲线外标法定量。水杨酸的响应值在1.25~20.00 ng/m L范围内具有良好的线性关系,相关系数(R~2)为0.998 4;赤霉酸的响应值在10~1000 ng/m L范围内呈良好的线性关系,相关系数(R~2)为0.993 3,在3个加标含量条件下,水杨酸(1.25、2.50、5.00μg/kg)、赤霉酸(10.0、50.0、100.0μg/kg)的回收率分别为87.6%~95.3%和83.8%~96.5%,相对标准偏差不高于6.9%,方法的检出限分别为0.01、0.15ng/m L。

Simultaneous Determination of Salicylic Acid and Gibberellic Acid in Tomato by High Performance Liquid Chromatography Tandem Mass Spectrometry

A sensitive and selective method was developed using high performance liquid chromatography-positive ion mode
electrospray ionization-tandem mass spectrometry (HPLC-MS/MS) for the simultaneous determination of salicylic acid
(SA) and gibberellic acid (GA3) in tomato. The analytes were extracted with a mixture of acetic acid and acetonitrile; the
extract was purified with solid-phase extraction (SPE) on an octadecylsilane (C18) column. Then SA and GA3 in the extract
were separated on a reversed phase C18 column using a gradient elution program with 0.5% formic acid–methanol as the
mobile phase. Qualitative analysis was performed with electrospray ionization in anion mode (ESI-) under multiple reaction
monitoring (MRM) mode. The matrix-matched calibrations were used for quantitation. The calibration curves showed a
good linearity in the concentration range of 1.25–20.00 and 10–1 000 ng/mL for SA and GA3, with correlation coefficients (R2)
of 0.998 4 and 0.993 3, respectively. The average recoveries of SA and GA3 in tomato were in the range of 87.6%–95.3%
and 83.8%–96.5% at three spiked concentration levels, and relative standard deviations (RSD, n = 3) were less than 6.9%.
The limits of quantitation (LOQ) for SA and GA3 were 0.01, and 0.15 (ng/mL), respectively. The method could be used for
the rapid and accurate detection of these hormones in tomato.