超高效液相色谱-串联质谱法快速测定豆芽中12种植物生长调节剂的含量

Rapid Determination of 12 Plant Growth Regulators in Bean Sprouts by Ultra-High Performance Liquid Chromatography-Tandem Mass Spectrometry

提出了超高效液相色谱-串联质谱法(UHPLC-MS/MS)快速测定豆芽中12种植物生长调节剂的方法。样品5.00 g用体积比1∶99的乙酸-乙腈混合液10 mL提取,离心后取上清液1.0 mL,经QuEChERS净化。以Waters Acquity UPLC?HSS T3色谱柱为固定相,以不同体积比的乙腈和含0.1%(体积分数)甲酸的5 mmoL·L^(-1)甲酸铵溶液的混合液为流动相进行梯度洗脱。质谱分析中采用电喷雾正、负离子源和多反应监测模式检测,基质匹配外标法定量。12种植物生长调节剂的质量分数与其峰面积在一定范围内呈线性关系,检出限(3S/N)为0.60~6.0μg·kg-1。按标准加入法进行回收试验,测得回收率为70.0%~110%,测定值的相对标准偏差(n=6)均小于10%。按此方法分析了32份豆芽样品,检出率为31.25%。

A method was proposed for the rapid determination of 12 plant growth regulators in bean sprouts by ultra-high performance liquid chromatography-tandem mass spectrometry(UHPLC-MS/MS).The sample(5.00 g)was extracted with 10 mL of a mixture of acetic acid and acetonitrile at volume ratio of 1∶99.After centrifugation,1.0 mL of the supernatant was purified by QuEChERS.Waters Acquity UPLC?HSS T3 chromatographic column was used as stationary phase,and the mixtures of acetonitrile and 5 mmol·L^(-1)ammonium formate containing 0.1%(φ)formic acid at different volume ratios were used as mobile phase for gradient elution.ESI+,ESI-and the mode of multireaction monitoring(MRM)were adopted in MS/MS,and matrix matching external standard method was used for quantitative analysis.The results showed that linear relationships between values of mass fraction and peak area of 12 plant growth regulators were found in the definite ranges,with detection limits(3 S/N)in the range of 0.60-6.0μg·kg-1.Test for recovery was made by standard addition method,giving results in the range of 70.0%-110%,and RSDs(n=5)of the determined values less than 10%.This method was used to analyze 32 samples bean sprouts,and the detection rate was 31.25%.