同位素稀释-气相色谱-质谱法测定食用植物油中总氯丙醇脂肪酸酯 |
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引用本文: | 李珊,易青,苗虹,吴永宁. 同位素稀释-气相色谱-质谱法测定食用植物油中总氯丙醇脂肪酸酯[J]. 分析化学, 2016, 0(6): 893-900. DOI: 10.11895/j.issn.0253-3820.150718 |
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作者姓名: | 李珊 易青 苗虹 吴永宁 |
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作者单位: | 国家食品安全风险评估中心 卫生部食品安全风险评估重点实验室,北京,100021 |
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基金项目: | 国家重点基础研究发展计划(No.2012CB20804)项目资助This work was supported by the State Key Development Program for Basic Research of China (2012CB720804) |
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摘 要: | 建立了食用植物油中总氯丙醇脂肪酸酯(氯丙醇酯)的同位素稀释-气相色谱-质谱(GC-MS)检测方法。样品经甲醇钠-甲醇溶液水解,硅藻土小柱净化,七氟丁酰咪唑(HFBI)衍生后,GC-MS 检测,同位素内标法定量。3-MCPD 酯、2-MCPD 酯、1,3-DCP 酯和2,3-DCP 酯在0.050~2.000 mg/ L 浓度范围内,均呈良好线性相关,相关系数(R)均大于0.9995。3-MCPD 酯、2-MCPD 酯、1,3-DCP 酯和2,3-DCP 酯的检出限分别为0.015,0.015,0.030和0.030 mg/ kg,定量限分别为0.050,0.050,0.100和0.100 mg/ kg。以空白特级初榨橄榄油为空白基质的加标回收实验的平均回收率为87.0%~110.5%,相对标准偏差(RSD)均小于10.1%。在74份食用植物油样品中,3-MCPD 酯、2-MCPD 酯和1,3-DCP 酯的检出率分别为94.6%,63.5%和5.4%,未检出2,3-DCP 酯;3-MCPD 酯、2-MCPD 酯和1,3-DCP 酯的含量分别在未检出(ND)~10.646 mg/ kg、ND ~3.617 mg/ kg 和ND ~0.089 mg/ kg 之间。本方法简便、准确、可靠,适用于食用植物油中总氯丙醇酯的测定。
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关 键 词: | 食用植物油 氯丙醇脂肪酸酯 气相色谱-质谱法 同位素稀释技术 |
Determination of Total Fatty Acid Esters of Chloropropanols in Edible Vegetable Oils by Gas Chromatography-Mass Spectrometry |
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Abstract: | A method was established for the simultaneous determination of the total fatty acid esters of chloropropanols in edible oils by gas chromatography-mass spectrometry combined with isotope dilution technology. The samples were hydrolyzed with sodium methylate-methanol, and then purified by diatomite cartridge. After being derivatized with heptafluorobutyrylimidazole ( HFBI ), the target analytes were determined by GC-MS with the deuteriumchloropropanols esters as the internal standards. An excellent linear correlation in the range of 0. 050-2. 000 mg / L was acquired for 3-monochloropropane-1,2-diol (3-MCPD) esters, 2-MCPD esters, dichloropropan-2-ol (1,3-DCP) esters and 2,3-dichloropropan-1-ol (2,3-DCP) esters, with all the correlation coefficients (r) higher than 0. 9995. The limits of detection (LODs) for 3-MCPD esters, 2-MCPD esters, 1,3-DCP esters and 2,3-DCP esters were 0. 015, 0. 015, 0. 030, and 0. 030 mg / kg, respectively, and the limits of quantitation (LOQ) were 0. 050, 0. 050, 0. 100, and 0. 100 mg / kg, respectively. The average spike recoveries of the four kinds of chloropropanols esters in blank extra virgin olive oil matrix were typically in a range of 87. 0% -110. 5% with the relative standard deviations (RSDs) less than 10. 1% . The detection rates of 3-MCPD esters, 2-MCPD esters, 1,3-DCP esters and 2,3-DCP esters in 74 edible oil samples were 94. 6% , 63. 5% , 5. 4% , and 0% , respectively. The contamination levels of 3-MCPD esters, 2-MCPD esters and 1,3-DCP esters were in the range of not detected (ND) to 10. 646 mg / kg, ND to 3. 617 mg / kg and ND to 0. 089 mg / kg, respectively. This method is accurate and rugged for the simultaneous determination of total fatty acid esters of chloropropanols in edible vegetable oils. |
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Keywords: | Edible vegetable oil Fatty acid esters of chloropropanols Gas chromatography-mass spectrometry Isotope dilution technology |
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