高效液相色谱-串联质谱法测定豆芽中4-氯苯氧乙酸钠

Determination of Sodium parachlorophenoxy in Bean Sprouts by HPLC-MS/MS

中文关键词:  高效液相色谱-质谱联用  加热电喷雾电离  豆芽  4-氯苯氧乙酸钠

英文关键词:High Performance Liquid Chromatography-Mass Spectrometry  Heating-

中文摘要:

      目的 建立了豆芽中4-氯苯氧乙酸钠的液相色谱-串联质谱测定方法。方法豆芽样品均质后以0.01 mol/L 氢氧化钠溶液提取，提取液经酸化后再用乙酸乙酯萃取，收集经离心分层的有机相，浓缩后用甲醇溶解进行测定分析。以甲醇和0.1% 甲酸（FA）水溶液为流动相，采用Hypersil GOLD aQ (100 mm×2.1 mm，3 μm)色谱柱分离，电喷雾电离负离子条件下以选择反应监测模式（SRM）检测。结果 该方法检出限0.005 mg/kg，在0~0.1 μg/mL范围内具有良好线性，相关系数为0.9998。回收率为79.1~104.7%，相对标准偏差低于5% (n= 6)。结论 该方法前处理简单快速，定性准确，灵敏度好，适用于豆芽中4-氯苯氧乙酸钠的残留检测。

英文摘要:

      Objective An analytical method was established for determination of Sodium parachlorophenoxy (4-CPANa) in bean sprouts by High Performance Liquid Chromatography Tandem Mass Spectrometry (HPLC-MS/MS). Methods The soybean sample was extracted with 0.01 mol/L sodium hydroxide solution, and the extracting solution was recovered by diethyl ether in acidic condition. After centrifugation, the organic phase was concentrated completely and re-dissolved with methanol. The sample was separated by Hypersil GOLD aQ Column (100 mm×2.1 mm, 3 μm) with methanol and 0.1% FA aqueous as mobile phase. The remnant was detected by MS/MS using H-ESI technology (negative ion mode) and SRM detection mode. Results The detection limit was 0.002 mg/kg and the linear range was 0~0.1 μg/mL with correlation coefficient(r2=0.9998). The average recoveries were between 79.1%~104.7% with relative standard deviation (RSD) less than 5% (n=6). Conclusion This analytical method is sample, rapid, and high sensitive, it can be accurate qualitative and used for the rapid detection of Sodium parachlorophenoxy.