盐析辅助液液萃取-超高效液相色谱-串联质谱法快速测定糕点中14种生物碱

Rapid determination of 14 kinds of alkaloids in pastries by salting-out assisted liquid-liquid extraction with ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  盐析辅助液液萃取  超高效液相色谱-串联质谱法  生物碱  糕点

英文关键词:salting-out assisted liquid-liquid extraction  ultra performance liquid chromatography-tandem mass spectrometry  alkaloids  pastries

中文摘要:

      目的 建立一种应用盐析辅助液液萃取前处理技术结合超高效液相色谱-串联质谱法快速测定糕点中14种常见有毒生物碱的分析方法。方法 样品加水超声处理后, 在碱性条件下(pH=11), 用乙腈提取, 加入氯化钠盐析分层。取乙腈相氮吹至干后用40%甲醇水溶液复溶, 使用0.1%甲酸-5 mmol/L甲酸铵的水溶液和乙腈为流动相, 在C18色谱柱(100 mm×2.1 mm, 2.5 μm)上通过梯度洗脱实现目标物分离, 在串联质谱正离子多反应监测模式下进行检测, 溶剂标准曲线外标法定量。结果 14种生物碱在0.5~100.0 ng/mL的范围内具有良好的线性关系, 相关系数均≥0.999, 检出限和定量限范围分别为0.1~2.2 μg/kg和0.3~7.1 μg/kg。在8.00、50.00和200.00 μg/kg的加标浓度下, 14种生物碱的平均回收率为76.3%~105.7%, 相对标准偏差为1.2%~9.8% (n=6)。结论 本方法简单、快速、准确, 能满足糕点中14种生物碱的快速筛查和定量分析, 可用于疑似生物碱中毒的应急事件处理。

英文摘要:

      Objective To establish an analytical method for the rapid determination of 14 kinds of common toxic alkaloids in pastries using salting-out assisted liquid-liquid extraction pretreatment combined with ultra performance liquid chromatography-tandem mass spectrometry. Methods The samples were ultrasonicated with water, extracted with acetonitrile under alkaline conditions (pH=11) and separated by adding sodium chloride for salting-out. The acetonitrile phase was dried by nitrogen blowing and then redissolved with 40% methanol aqueous solution. The separation of the targets was achieved by gradient elution on C18 column (100 mm×2.1 mm, 2.5 μm) using 0.1% formic acid-5 mmol/L ammonium formate aqueous solution and acetonitrile as the mobile phases, and the targets were detected by tandem mass spectrometry positive ion multiple reaction monitoring mode, and quantified by external standard method with solvent standard curve. Results The 14 kinds of alkaloids showed good linearity in the range of 0.5–100.0 ng/mL with the correlation coefficients greater than or equal to 0.999. The ranges for limits of detection and the limits of quantitation were 0.1–2.2 μg/kg and 0.3–7.1 μg/kg. The average recoveries for the 14 kinds of alkaloids at spiked concentrations of 8.00, 50.00 and 200.00 μg/kg range from 76.3%-105.7% with the relative standard deviations of 1.2%-9.8% (n=6). Conclusion The method is simple, quick and accurate, which can meet the requirements of rapid screening and quantitative analysis of 14 kinds of alkaloids in pastries, and can be used for emergency incident management of suspected alkaloid poisoning.