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    大气压气相色谱-串联质谱法测定食用油中37种脂肪酸的含量

    Determination of 37 Fatty Acids in Edible Oils by Atmospheric Pressure Gas Chromatography-Tandem Mass Spectrometry

    • 摘要: 为提高气相色谱-串联质谱法检测食用油中多种脂肪酸的灵敏度和定性定量效果,进行了题示研究。参考GB 5009.168—2016进行样品前处理。取1 g混合均匀的食用油样品,加入含2%(质量分数)氢氧化钠的甲醇溶液8 mL,于(80±1) ℃加热回流至油滴消失。在回流冷凝器上端加入7 mL 15%(体积分数)三氟化硼甲醇溶液,于(80±1) ℃加热回流2 min。冷却至室温,加入10 mL正庚烷,振摇2 min,再加入3 mL饱和氯化钠溶液,静置分层。吸取上层正庚烷提取溶液5 mL,加入3 g无水硫酸钠,振摇1 min,静置5 min,上层溶液采用大气压气相色谱-串联质谱法测定。37种脂肪酸甲酯以CD-2560毛细管色谱柱在程序升温条件下分离,大气压气相色谱电离源电离,多反应监测(MRM)模式检测,外标法定量。结果显示:37种脂肪酸甲酯在一定范围内和峰面积呈线性关系,相关系数不小于0.999 0,检出限(3S/N)为0.1~1.3 mg·kg-1。按照标准加入法进行回收试验,回收率为80.0%~116%,测定值的相对标准偏差(n=6)均小于10%。方法用于5种食用油样品的分析,饱和脂肪酸检出量最高的为猪油(54.450 7%),其余依次为玉米油(22.970 2%)、橄榄油(20.556 1%)、核桃油(11.367 4%)、菜籽油(9.530 8%);不饱和脂肪酸检出量最高的为菜籽油(90.463 0%),其余依次为核桃油(88.626 8%)、橄榄油(79.436 0%)、玉米油(77.025 0%)、猪油(45.547 2%)。

       

      Abstract: The study mentioned by the title was conducted to improve the sensitivity and qualitative and quantitative effects of gas chromatography-tandem mass spectrometry for detecting various fatty acids in edible oils. Referring to GB 5009.168-2016 for sample pretreatment, 1 g of evenly mixed edible oil sample was taken, and 8 mL of methanol solution containing 2% (mass fraction) sodium hydroxide was added. The mixed solution was heated by reflux at (80±1) °C until the oil droplets disappeared. Then 7 mL of 15% (volume fraction) boron trifluoride methanol solution was added into the upper end of the reflux condenser, and the mixed solution was heated by reflux at (80±1) °C for 2 min. After cooling to room temperature, 10 mL of n-heptane was added, and the mixed solution was shaken for 2 min. Then 3 mL of saturated sodium chloride solution was added, and the mixture was settled for stratification. The 5 mL of the upper n-heptane extract was taken, and 3 g of anhydrous sodium sulfate was added. The mixture was shaken for 1 min, and settled for 5 min, and the upper solution was taken and determined by atmospheric pressure gas chromatography-tandem mass spectrometry. The 37 fatty acid methyl esters were separated on CD-2560 capillary chromatographic column under programmed temperature conditions, ionized by atmospheric pressure gas chromatography ionization source, detected in multiple reaction monitoring (MRM) mode, and quantified by external standard method. It was shown that linear relationships between the mass centrations and peak areas of 37 fatty acid methyl esters were kept in definite ranges, with correlation coefficients not less than 0.999 0, and detection limits (3S/N) in the range of 0.1-1.3 mg·kg-1. Test for recovery was made according to the standard addition method, giving recoveries in the range of 80.0%-116%, and RSDs (n=6) of the determined values were less than 10%. The proposed method was used for the analysis of five types of edible oil samples. The highest detection amount of saturated fatty acids was found in lard (54.450 7%), followed by corn oil (22.970 2%), olive oil (20.556 1%), walnut oil (11.367 4%), and rapeseed oil (9.530 8%). The highest detection amount of unsaturated fatty acids was found in rapeseed oil (90.463 0%), followed by walnut oil (88.626 8%), olive oil (79.436 0%), corn oil (77.025 0%), and lard (45.547 2%).

       

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