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  被引量:12

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

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作  者:唐莉娟[1] 谭婷[1] 万益群[1,2] 

机构地区:[1]南昌大学分析测试中心,江西南昌330047 [2]南昌大学食品科学与技术国家重点实验室,江西南昌330047

出  处:《食品科学》2012年第14期136-141,共6页Food Science

基  金:国家自然科学基金地区科学基金项目(20765002;20965005);江西省科技支撑计划项目(2008BB22400);南昌大学食品科学与技术国家重点实验室目标导项目(SKLF-MB-201002);南昌大学食品科学与技术国家重点实验室自由探索项目(SKLF-TS-200918)

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。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 × 4.6mm, 5μm) 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 spectromeWic 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 ~t g/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.

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 

分 类 号:O657.7[理学—分析化学]

 

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