顶空箭形固相微萃取-气相色谱-质谱法测定食盐中9种短链脂肪酸

Determination of 9 kinds of short-chain fatty acids in salt by headspace solid phase microextraction arrow-gas chromatography-mass spectrometry

中文关键词:  食盐  短链脂肪酸  顶空固相微萃取  气相色谱质谱

英文关键词:salt  short-chain fatty acids  headspace solid phase microextraction  gas chromatography-mass spectrometry

中文摘要:

      目的 建立顶空箭形固相微萃取-气相色谱-质谱法测定食盐中短链脂肪酸的定性和定量分析方法。方法 在食盐样品中加入磷酸溶液, 基于箭形固相微萃取技术对短链脂肪酸进行萃取富集, 探究了萃取头、萃取温度、萃取时间、孵育时间对萃取效果的影响, 目标物用气相色谱-质谱法检测, 外标法定量。结果 萃取头100 μm Polyacrylate对短链脂肪酸有较好的选择性, 在萃取温度40 ℃、时间30 min, 解析时间5 min, 孵育时间20 min的条件下, 9种短链脂肪酸线性关系良好, 相关系数大于0.995, 检出限为0.25~25.00 μg/kg, 回收率为92.2%~100.1%, 相对标准偏差为1.4%~9.4%。结论 本研究建立的食盐中短链脂肪酸的分析方法样品制备简单, 灵敏度高, 回收率和稳定性好, 适用于食盐中短链脂肪酸的检测。

英文摘要:

      Objective To establish a qualitative and quantitative analytical method for determination of short-chain fatty acids in table salt using headspace solid phase microextraction arrow-gas chromatography-mass spectrometry. Methods A phosphoric acid solution was added to the salt samples, and the headspace solid phase microextraction arrow technique was employed to extract and enrich the short-chain fatty acids. The effects of extraction fiber, extraction temperature, extraction time, and incubation time on the extraction efficiency were investigated. The target compounds were detected by gas chromatography-mass spectrometry and quantified using the external standard method. Results The 100 μm Polyacrylate extraction fiber demonstrated good selectivity for short-chain fatty acids. Under optimal conditions (extraction temperature of 40 °C, extraction time of 30 min, desorption time of 5 min and incubation time of 20 min), the method showed excellent linearity for 9 kinds of short-chain fatty acids, with correlation coefficients greater than 0.995. The limits of detection ranged from 0.25 to 25.00 μg/kg, the recovery rates were between 92.2% and 100.1%, and the relative standard deviations ranged from 1.4% to 9.4%. Conclusion The established method for analyzing short-chain fatty acids in table salt is characterized by simple sample preparation, high sensitivity, good recovery rates and stability, making it suitable for the detection of short-chain fatty acids in table salt.