棉籽油及其副产品中矮壮素与缩节胺的HPLC-MS/MS检测方法优化

Optimized detection method for chlormequat and mepiquat in cotton seed oil and its by-products using high performance liquid chromatography-mass spectrometry

中文关键词:  棉籽油  棉粕  矮壮素  缩节胺

英文关键词:cottonseed oil  cottonseed meal  chlormequat  mepiquat

中文摘要:

      目的 建立棉籽油及其副产品中矮壮素和缩节胺的高效液相色谱-串联质谱检测方法。方法 样品经水或含40%乙腈的缓冲溶液(v:v)提取后, 过0.22 μm滤膜净化, 再经Agilent ZORBAX RX-SIL (100 mm×3.0 mm,1.8 μm)色谱柱分离; 流动相以0.2%甲酸+10 mmol/L乙酸铵水为A液, 甲醇为B液; 以流速0.4 mL/min洗脱。电喷雾正离子模式(ESI ), 多反应监测模式(MRM)检测。结果 使用该方法检测矮壮素和缩节胺在0.2~0.5 μg/L范围内呈良好线性。在1.0、5.0、10.0 mg/kg 三个加标水平回收率分别为92.2%~98.7%之间, 相对标准偏差在1.9%~6.7%之间。结论 说明此方法灵敏度高、定性准确、具有比较好的加标回收率, 可满足检测要求。

英文摘要:

      Objective To establish a detection method of chlormequat and mepiquat from cottonseed oil and by-products by high performance liquid chromatography-mass spectrometry (HPLC-MS/MS). Methods The samples were extracted by water or containing 40% acetonitrile (v:v) buffer solution, and purified by 0.22 μm filter membrane, and separated in Agilent ZORBAX RX-SIL column (100 mm×3.0 mm, 1.8 μm). The mobile phase was divided into A solution with 0.2% formic acid +10 mmol/L ammonium acetate aqueous, B solution with methanol, to elute of a flow rate at 0.4mL/min. Electrospray ionization in the positive ion mode (ESI ), multiple reaction monitoring mode (MRM) detection. Results It showed there was a good linearity in the range of 0.2~0.5 μg/L for chlormequat and mepiquat, the recovery of standard addition was 92.2%~98.7%, the relative standard deviation was 1.9~6.7% in 1, 5, and 10.0mg/kg levels. Conclusion The method could better meet the test requirement in sensitive, accurate, and the recovery rate.