超声波提取-高效液相色谱/电喷雾离子化质谱法测定白萝卜中植物生长调节剂

食品科学 ›› 2012, Vol. 33 ›› Issue (14): 136-141.

超声波提取-高效液相色谱/电喷雾离子化质谱法测定白萝卜中植物生长调节剂

唐莉娟1，谭婷1，万益群1,2,*

1.南昌大学分析测试中心 2.南昌大学食品科学与技术国家重点实验室

收稿日期:2011-06-30 修回日期:2012-05-26 出版日期:2012-07-25 发布日期:2012-07-27
通讯作者: 万益群 E-mail:yqwanoy@sina.com
基金资助:
国家自然科学基金项目;江西省科技支撑计划项目;南昌大学食品科学与技术国家重点实验室目标导向项目;南昌大学食品科学与技术国家重点实验室自由探索项目

Determination of Plant Growth Regulators in Radish by Ultrasound-Assisted Extraction and Liquid Chromatography-Electrospray Ionization Mass Spectrometry

Received:2011-06-30 Revised:2012-05-26 Online:2012-07-25 Published:2012-07-27

摘要/Abstract

摘要： 建立白萝卜中2-萘氧乙酸、2,4-D、萘乙酸3种植物生长调节剂同时测定的高效液相色谱-电喷雾离子化质谱分析方法。采用Diamonsil C18色谱柱(250mm×4.6mm，5μm)，以V(0.01mol/L甲酸-甲酸铵缓冲溶液，pH4):V(甲醇)=30:70为流动相，流速为0.7mL/min，采用选择负离子监测模式对各物质的定量离子进行监测。结果表明，3种植物生长调节剂在8min内实现快速基线分离，且在0.01～10μg/mL范围内线性关系良好。2-萘氧乙酸、2,4-D以及萘乙酸的方法检出限分别为0.0018、0.004、0.003mg/kg。在0.01、0.05mg/kg和0.50mg/kg三个水平上对白萝卜进行加标回收实验，平均回收率在77.56%～105.08%之间，相对标准偏差在3.48%～15.88%之间。该方法用于白萝卜中植物生长调节剂的检测，结果良好。

关键词: 高效液相色谱-电喷雾离子化质谱, 超声波提取, 植物生长调节剂, 白萝卜

Abstract: A new method for the determination of plant growth regulators including 2-naphthoxyacetic acid, 2,4-dicholrophenoxyacetic acid and 1-naphthlcetic acid in radish was developed by liquid chromatography-electrospray ionization mass spectrometry (LC-ESI/MS). The chromatographic separation was performed on a Diamonsil C18 column (250 mm× 4.6 mm, 5 μm) by using a mobile phase made up of 0.01 mol/L formic acid-ammonium buffer solution (pH 4) and methanol (30:70, V/V) at a flow rate of 0.7 mL/min. The mass spectrometric quantitative analysis was based on selective ionic measurement by electro-spray ionization in the negative ion mode. Baseline separation was achieved for three plant growth regulators within 8 min. Good linearity was observed in the range of 0.01－10 μg/mL for all of them. The detection limit at a signal to noise ratio of 3 was 0.0018 mg/kg for 2-naphthoxyacetic acid, 0.004 mg/kg for 2,4-dicholrophenoxyacetic acid and 0.003 mg/kg for 1-naphthlcetic acid, respectively. Under optimal conditions, the average recovery rate and relative standard deviation were 77.56%－105.08% and 3.48%－15.88% at spike levels of 0.01, 0.05 mg/kg and 0.50 mg/kg, respectively. Therefore, this method is suitable for the determination of plant growth regulators in radish.

Key words: liquid chromatography-electrospray ionization mass spectrometry (LC-ESI/MS), ultrasound-assisted extraction, plant growth regulator, radish

中图分类号:

Q946.885

唐莉娟1，谭婷1，万益群1,2,*. 超声波提取-高效液相色谱/电喷雾离子化质谱法测定白萝卜中植物生长调节剂[J]. 食品科学, 2012, 33(14): 136-141.

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