高效液相色谱-串联质谱同时测定豆芽中8种生长调节剂残留量

Determination of Eight Growth Regulators in Bean Sprouts by HPLC-MS/MS

建立了高效液相色谱-串联质谱法同时测定豆芽中6-苄基腺嘌呤、4-氯苯氧乙酸、2,4-D、赤霉素、1-萘乙酸、2-萘氧乙酸、吲哚乙酸、噻苯隆等8种生长调节剂残留量的方法。样品用含1%甲酸甲醇溶液提取,HLB固相萃取柱净化后,经C18色谱柱分离,乙腈-10 mmol/L乙酸铵（含0.1%甲酸）流动相梯度洗脱,串联三重四级杆质谱仪电喷雾负离子多反应监测（MRM）模式下进行检测。结果表明,8种生长调节剂在1～1000μg/L范围内线性关系良好;方法定量限（S/N=10）为0.03～50μg/kg;添加水平为5、10、20μg/kg（萘乙酸和吲哚乙酸为50、100、200μg/kg）时,平均回收率在71.5%～92.3%之间;相对标准偏差（RSD,n=6）为4.6%～13.5%。方法简单快速,灵敏度高,成功应用于市场上绿豆芽和黄豆芽的检测。

A high performance liquid chromatography-tandem mass spectrometry（HPLC-MS/MS） method was developed for the determination of 8 kinds of plant growth regulators such as 6-benzylaminopurine, 4-chlorophenoxyacetic acid, 2,4-D, gibberellin acid, 1-naphthlcetic acid, 2-naphthoxyacetic acid, indole-3-acetic acid and thidiazuron residue in bean sprouts. The samples were extracted with methanol containing 1 % formic acid solution, cleaned up with HLB solid-phase extraction column. The chromatographic analysi was carried out on a C18 column with acetonitrile and 10 mmol/L ammonium acetate（containing 0.1 % formic acid） solution as the mobile phase in gradient elution program. The extract was analyzed by HPLC-MS/MS on anion multiple reaction monitoring（MRM） mode. The results showed that 8 kinds of growth regulators in 1～1000 μg/L range with good line. The limits of quantitation（S/N=10） was 0.03～50 μg/kg. At three spiked concentration levels of 5, 10 and 20 μg/kg（1-naphthlcetic acid and indole-3-acetic acid for 50, 100, 200 μg/kg）, the average recovery was 71.5 %～92.3 % with relative standard deviation（RSD, n=6） was 4.6 %～13.5 %. The method is simple and rapid, high sensitivity, and successfully applied testing growth regulators in mungbean sprout and yellow bean sprouts from the market.