气相色谱-串联质谱法同时测定大米中13种香精成分

Simultaneous determination of 13 kinds of flavor compounds in rice by gas chromatography-tandem mass spectrometry

中文关键词:  香精  大米  气相色谱-串联质谱法

英文关键词:flavor compounds  rice  gas chromatography-tandem mass spectrometry

中文摘要:

      目的 建立气相色谱-串联质谱法(gas chromatography-tandem mass spectrometry, GC-MS/MS)同时测定大米中13种香精成分的方法。方法 样品经25%乙醇溶液提取后, 采用二氯甲烷进行液液萃取, 取下层二氯甲烷层经无水硫酸钠过滤并高速离心后, 以DB-5MS (30 m×0.25 mm, 0.25 μm)色谱柱分离, 经程序升温分离, 在多反应监测(multiple reaction monitoring, MRM)模式下测定, 以基质提取液配制标准曲线外标法定量。结果 13种香精成分在各自浓度范围内线性关系良好, 相关系数均大于0.990, 检出限为0.5~5.0 μg/kg, 定量限为2.0~20.0 μg/kg, 以大米为方法学考察基质进行3个浓度水平加标回收实验, 平均回收率为81.55%~115.10%, 相对标准偏差为1.6%~6.3%。结论 该方法灵敏度高, 定性、定量准确, 简便高效, 可适用于大米中13种香精成分的同时检测要求。

英文摘要:

      Objective To establish a method for the simultaneous determination of 13 kinds of flavor compounds in rice by gas chromatography-tandem mass spectrometry (GC-MS/MS). Methods The sample was extracted with 25% ethanol solution, followed by liquid-liquid extraction using dichloromethane. The lower dichloromethane phase was filtered through anhydrous sodium sulfate and subjected to high-speed centrifugation. Separation was performed on a DB-5MS column (30 m×0.25 mm, 0.25 μm) with a programmed temperature. Detection was carried out under multiple reaction monitoring (MRM) mode, and quantification was achieved via the external standard method with calibration curves prepared using matrix-matched extract. Results All 13 kinds of flavor compounds showed good linear relationships within their respective concentration ranges, with correlation coefficients greater than 0.990. The limits of detection and the limits of quantitation were 0.5–5.0 μg/kg and 2.0–20.0 μg/kg, respectively. Spike recovery experiments were conducted at 3 different levels in rice matrices, and the average recoveries were in the range of 81.55% to 115.10%, with the relative standard deviations varying from 1.6% to 6.3%. Conclusion The developed method features high sensitivity, accurate qualitative and quantitative results, simplicity and high efficiency, and is suitable for the simultaneous determination of 13 kinds of flavor compounds in rice.