全自动SPE-HPLC-DAD法测定熟肉制品中15种合成色素
|
摘要
利用全自动固相萃取-高效液相色谱技术,建立了熟肉制品中15种合成色素的高通量检测方法.样品经乙醚除脂后,用乙醇-水-氨水(70+30+1)溶液进行2遍提取,合并,浓缩,沉淀后取上清液使用全自动固相萃取仪进行固相萃取,洗脱液浓缩定容后进HPLC-DAD进行检测,采用外标法定量.15种色素在0. 05～20μg/mL的范围内线性关系良好(r> 0. 999),定量限为0. 02～0. 12 mg/kg.进行1～10倍定量限水平的添加回收试验,回收率范围为72. 05～99. 39%,相对标准偏差为0. 36～9. 23%.该方法在节约成本和缩短检测周期方面具有很大的优势.
A detection method of 15 kinds of synthetic pigments residues in cooked meat products is established by using the full-automatic solid-phase-extraction( SPE) and high performance liquid chromatography( HPLC). After defatted with ether,the sample is extracted twice with ethanol-water-ammonia( 70 + 30 + 1) solution,combined,concentrated,and precipitated. The full-automatic solid-phase extractor is used for solid-phase extraction,and the eluent is concentrated,and then detected by HPLC-DAD. External standard method is used for quantification. The method exhibites excellent linearity over a range of 0. 05-20 μg/mL( r > 0. 999). The recovery rate,LOQ,and relative standard deviation( RSD) are 72. 05%-99. 39 %,0. 02-0. 12 mg/kg,0. 36%-9. 23 %,respectively.This method has great advantages in reducing the cost and shortening the detection period.
A detection method of 15 kinds of synthetic pigments residues in cooked meat products is established by using the full-automatic solid-phase-extraction( SPE) and high performance liquid chromatography( HPLC). After defatted with ether,the sample is extracted twice with ethanol-water-ammonia( 70 + 30 + 1) solution,combined,concentrated,and precipitated. The full-automatic solid-phase extractor is used for solid-phase extraction,and the eluent is concentrated,and then detected by HPLC-DAD. External standard method is used for quantification. The method exhibites excellent linearity over a range of 0. 05-20 μg/mL( r > 0. 999). The recovery rate,LOQ,and relative standard deviation( RSD) are 72. 05%-99. 39 %,0. 02-0. 12 mg/kg,0. 36%-9. 23 %,respectively.This method has great advantages in reducing the cost and shortening the detection period.
引文
[1]张彦青，李伟，李亚茹，等．食用合成色素检测方法研究进展及其发展前景[J]．山东化工，2015,44(11):40-41.
[2]李翱楠，赫春香．示差脉冲极谱法测定柠檬黄[J]．广州化工，2011,39(21):112-114.
[3]王丽芳，丁晓静，解娜，等．毛细管电泳法测定糖果及调制酒中10种人工合成色素[J]．食品科学，2014,35(14):145-150.
[4]毕小玲，宋娟，庄晓洪，等．固相萃取-HPLC法检测熟肉制品中合成色素[J]．食品研究与开发，2017,38(5):180-183.
[5]黄方取，杨朝琳，严继东．固相萃取-高效液相色谱法测定肉制品中8种人工合成色素[J]．中国卫生检验杂志，2016,26(6):800-802.
[6] YANG Y,ZHANG J,SHAO B. Quantitative analysis of fourteen synthetic dyes in jelly and gummy candy by ultra performance liquid chromatography[J]. Analytical Methods,2014,6(15):5872-5878.
[7] MAZDEH F Z,KHORRAMI A R,MORADIKHATOONABADI Z. Determination of 8 synthetic food dyes by solid phase extraction and reversed-phase high performance liquid chromatography[J]. Tropical Journal of Pharmaceutical Research,2016,15(1):173-181.
[8]胡青，林媛，张甦，等．超高效液相色谱-三重串联四级杆质谱法测定乌梅中19种深色染色色素[J]．食品安全质量检测学报，2016,7(7):2663-2670.
[9] MARTIN F,OBERSON J M,MESCHIARI M,MUNARI C. Determination of 18 water-soluble artificial dyes by LC-MS in selected Matrices[J]. Food Chemistry,2016,197:1249-1255
[10] KAUFMANN A. Combining UHPLC and high-resolution MS:a viable approach for the analysis of complex samples[J].Trends in Analytical Chemistry,2014,63:113-128.
[11]中华人民共和国国家质量监督检验检疫总局．SN/T3536—2013出口食品中酸性橙Ⅱ号的检测方法[S]．北京:中国标准出版社，2013.
[12]中华人民共和国国家卫生和计划生育委员会．GB5009. 35—2016食品安全国家标准食品中合成着色剂的测定[S]．北京:中国标准出版社，2016.
[13]江苏省卫生和计划生育委员会．DBS 32012-2016食品安全地方标准食品中喹啉黄的检测高效液相色谱法、液相色谱-质谱质谱法[S]．北京:中国标准出版社，2016.
[14]中华人民共和国国家卫生和计划生育委员会．GB2760—2014食品添加剂使用标准[S]．北京:中国标准出版社，2014.
[15]刘梅．高通量合成色素测定方法的建立及其在熟肉制品检测中的应用[D]．泰安:山东农业大学，2018.
[2]李翱楠，赫春香．示差脉冲极谱法测定柠檬黄[J]．广州化工，2011,39(21):112-114.
[3]王丽芳，丁晓静，解娜，等．毛细管电泳法测定糖果及调制酒中10种人工合成色素[J]．食品科学，2014,35(14):145-150.
[4]毕小玲，宋娟，庄晓洪，等．固相萃取-HPLC法检测熟肉制品中合成色素[J]．食品研究与开发，2017,38(5):180-183.
[5]黄方取，杨朝琳，严继东．固相萃取-高效液相色谱法测定肉制品中8种人工合成色素[J]．中国卫生检验杂志，2016,26(6):800-802.
[6] YANG Y,ZHANG J,SHAO B. Quantitative analysis of fourteen synthetic dyes in jelly and gummy candy by ultra performance liquid chromatography[J]. Analytical Methods,2014,6(15):5872-5878.
[7] MAZDEH F Z,KHORRAMI A R,MORADIKHATOONABADI Z. Determination of 8 synthetic food dyes by solid phase extraction and reversed-phase high performance liquid chromatography[J]. Tropical Journal of Pharmaceutical Research,2016,15(1):173-181.
[8]胡青，林媛，张甦，等．超高效液相色谱-三重串联四级杆质谱法测定乌梅中19种深色染色色素[J]．食品安全质量检测学报，2016,7(7):2663-2670.
[9] MARTIN F,OBERSON J M,MESCHIARI M,MUNARI C. Determination of 18 water-soluble artificial dyes by LC-MS in selected Matrices[J]. Food Chemistry,2016,197:1249-1255
[10] KAUFMANN A. Combining UHPLC and high-resolution MS:a viable approach for the analysis of complex samples[J].Trends in Analytical Chemistry,2014,63:113-128.
[11]中华人民共和国国家质量监督检验检疫总局．SN/T3536—2013出口食品中酸性橙Ⅱ号的检测方法[S]．北京:中国标准出版社，2013.
[12]中华人民共和国国家卫生和计划生育委员会．GB5009. 35—2016食品安全国家标准食品中合成着色剂的测定[S]．北京:中国标准出版社，2016.
[13]江苏省卫生和计划生育委员会．DBS 32012-2016食品安全地方标准食品中喹啉黄的检测高效液相色谱法、液相色谱-质谱质谱法[S]．北京:中国标准出版社，2016.
[14]中华人民共和国国家卫生和计划生育委员会．GB2760—2014食品添加剂使用标准[S]．北京:中国标准出版社，2014.
[15]刘梅．高通量合成色素测定方法的建立及其在熟肉制品检测中的应用[D]．泰安:山东农业大学，2018.