婴幼儿配方奶粉中缩水甘油脂肪酸酯含量的测定
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摘要
建立了气相色谱-质谱法测定婴幼儿配方奶粉中缩水甘油脂肪酸酯(GEs)含量的方法,并对水解时间、中和后溶液的酸度、氯代反应时间进行了优化。在最佳条件下进行方法学指标的验证,缩水甘油脂肪酸酯在16.9～507.6μg/L范围内呈现良好的线性关系(r>0.999),方法的检出限(3 S/N)为0.005 mg/kg(以奶粉中缩水甘油计),回收率为93.5%～103%,RSD为3.70%～5.75%(n=6)。该方法的准确度好、灵敏度高,适用于婴幼儿配方奶粉中缩水甘油脂肪酸酯含量测定。
A method for the determination of glycidyl fatty acid esters(GEs) in infant formula milk powder by gas chromatography-mass spectrometry(GC-MS) was established. The hydrolysis time,acidity of neutralized solution and chlorination reaction time were optimized. Under the optimized conditions,GEs showed a good linearity in rang of 16.9-507.6 μg/L(r>0.999). The detection limit(3 S/N)of GEs was 0.005 mg/kg(calculated by Gly in infant formula milk powder). The average recoveries for GEs were ranged from 93.5% to 103%,with the relative standard derivation(RSD)ranging from 3.70%to 5.75%(n=6). This method was successfully applied to analyze GEs in infant formula milk powder with good reproducibility and sensitivity.
A method for the determination of glycidyl fatty acid esters(GEs) in infant formula milk powder by gas chromatography-mass spectrometry(GC-MS) was established. The hydrolysis time,acidity of neutralized solution and chlorination reaction time were optimized. Under the optimized conditions,GEs showed a good linearity in rang of 16.9-507.6 μg/L(r>0.999). The detection limit(3 S/N)of GEs was 0.005 mg/kg(calculated by Gly in infant formula milk powder). The average recoveries for GEs were ranged from 93.5% to 103%,with the relative standard derivation(RSD)ranging from 3.70%to 5.75%(n=6). This method was successfully applied to analyze GEs in infant formula milk powder with good reproducibility and sensitivity.
引文
[1] 3-MCPD esters in food products,Workshop,ILSI Europe.Brussels,Belgium,February,2009..
[2] Federal Institute for Risk Assessment(BfR).Initial evaluation of the assessment of levels of glycidol fatty acid esters detected in refined vegetable fats(in German). BfR Opinion(2009).
[3]杨大进,李宁. 2017年国家食品污染物和有害因素风险工作手册[M].北京:中国标准出版社,2016.
[4]甘明,沈平,梁慧红,等.2012-2015年钦州市钦南区食品风险监测结果分析[J].现代预防医学,2017,44(12):2161-2164.
[5] Svejkovska B,Novotny O,Divinova V,et al. Esters of 3-chloropropane-1,2-diol in foodstuffs[J]. Czech Journal of Food Sciences,2004,22(5):190-196.
[6]刘国琴,尹诗琴,汪学德.气相色谱-质谱联用法测定食用油脂中的缩水甘油酯[J].现代食品科技,2016,32(05):289-294.
[7] DGF Standard Methods C-Ⅲ18(09). Ester-bound 3-chloropropane-1,2-diol(3-MCPD esters)and glycidol(glycidyl esters).Determination in fats and oils by GC-MS[S].
[8]宁柠.油脂工业中缩水甘油酯的产生规律及风险评估研究[D].华南理工大学,2015.
[9]刘京,张晖,王瑛瑶,等.液相色谱-质谱法测定食用植物油中缩水甘油酯的含量[J].食品工业科技,2014,35(15):308-311.
[10]吴永宁.现代食品安全科学[M].化学工业出版社,2003.
[11] Official Method Cd AOCS 29a-13,Approved 2017,2-and3-MCPD Fatty Acid Esters and Glycidol Fatty Acid Esters in Edible Oils and Fats by Acid Transesterification and GC/MS[S].
[12] Official Method Cd AOCS 29b-13,Approved 2017,2-and3-MCPD Fatty Acid Esters and Glycidol Fatty Acid Esters in Edible Oils and Fats by Alkaline Transesterification and GC/MS[S].
[13] Official Method Cd AOCS 29c-13,Approved 2017,2-and3-MCPD Fatty Acid Esters and Glycidol Fatty Acid Esters in Edible Oils and Fats by GC/MS(Difference Method)[S].
[14]胡守江,周静,张妮,等.同位素内标-气相色谱-质谱法测定婴幼儿配方乳粉中缩水甘油脂肪酸酯的含量[J].理化检验(化学分册),2018,54(07):7-13.
[15] DGF Standard Methods C-III 18(10):Fatty-acid-bound3-chloropropane-1,2-diol(3-MCPD)and 2,3-epoxipropane-1-ol(glycidol)Determination in oils and fats by GC/MS(Differential measurement)[S].
[16] GB 5413.3-2010.婴幼儿食品和乳品中脂肪的测定[S].
[2] Federal Institute for Risk Assessment(BfR).Initial evaluation of the assessment of levels of glycidol fatty acid esters detected in refined vegetable fats(in German). BfR Opinion(2009).
[3]杨大进,李宁. 2017年国家食品污染物和有害因素风险工作手册[M].北京:中国标准出版社,2016.
[4]甘明,沈平,梁慧红,等.2012-2015年钦州市钦南区食品风险监测结果分析[J].现代预防医学,2017,44(12):2161-2164.
[5] Svejkovska B,Novotny O,Divinova V,et al. Esters of 3-chloropropane-1,2-diol in foodstuffs[J]. Czech Journal of Food Sciences,2004,22(5):190-196.
[6]刘国琴,尹诗琴,汪学德.气相色谱-质谱联用法测定食用油脂中的缩水甘油酯[J].现代食品科技,2016,32(05):289-294.
[7] DGF Standard Methods C-Ⅲ18(09). Ester-bound 3-chloropropane-1,2-diol(3-MCPD esters)and glycidol(glycidyl esters).Determination in fats and oils by GC-MS[S].
[8]宁柠.油脂工业中缩水甘油酯的产生规律及风险评估研究[D].华南理工大学,2015.
[9]刘京,张晖,王瑛瑶,等.液相色谱-质谱法测定食用植物油中缩水甘油酯的含量[J].食品工业科技,2014,35(15):308-311.
[10]吴永宁.现代食品安全科学[M].化学工业出版社,2003.
[11] Official Method Cd AOCS 29a-13,Approved 2017,2-and3-MCPD Fatty Acid Esters and Glycidol Fatty Acid Esters in Edible Oils and Fats by Acid Transesterification and GC/MS[S].
[12] Official Method Cd AOCS 29b-13,Approved 2017,2-and3-MCPD Fatty Acid Esters and Glycidol Fatty Acid Esters in Edible Oils and Fats by Alkaline Transesterification and GC/MS[S].
[13] Official Method Cd AOCS 29c-13,Approved 2017,2-and3-MCPD Fatty Acid Esters and Glycidol Fatty Acid Esters in Edible Oils and Fats by GC/MS(Difference Method)[S].
[14]胡守江,周静,张妮,等.同位素内标-气相色谱-质谱法测定婴幼儿配方乳粉中缩水甘油脂肪酸酯的含量[J].理化检验(化学分册),2018,54(07):7-13.
[15] DGF Standard Methods C-III 18(10):Fatty-acid-bound3-chloropropane-1,2-diol(3-MCPD)and 2,3-epoxipropane-1-ol(glycidol)Determination in oils and fats by GC/MS(Differential measurement)[S].
[16] GB 5413.3-2010.婴幼儿食品和乳品中脂肪的测定[S].