牦牛乳制品中马尿酸和苯甲酸含量快速检测方法
|
摘要
利用高效液相色谱建立一种同时检测马尿酸和苯甲酸的快速检测方法,对不同沉淀剂、流动相、流速、回收率、最低检出限等进行讨论研究。结果表明:在C18(250 mm×4.6 mm,5.0μm)为分离柱,检测波长为230 nm,进液量为20μL条件下,流动相为甲醇-0.4%乙酸水溶液(50∶50,体积比),流速为0.9 mL/min时,马尿酸、苯甲酸在1μg/mL～100μg/mL范围内线性良好,最低检测浓度为0.038μg/mL,马尿酸平均回收率为96.79%～98.10%,相对标准偏差(relative standard deviation,RSD)为0.58%～1.07%,苯甲酸平均回收率为93.54%～98.99%,RSD为0.71%～1.19%。该方法灵敏度高、重现性好,定性定量分析效果佳。
A rapid method was established for simultaneous determination of hippuric acid and benzoic acid via high performance liquid chromatography. In this experiment,different precipitants,mobile phase,flow rate,recovery rate and minimum detection limit were discussed. The results showed that hippuric acid and benzoic acid ranged of 1 μg/mL-100 μg/mL had strong linearity in the detection and the minimum detection concentration was 0.038 μg/mL when methanol and 0.4 % acetic acid aqueous solution were used as mobile phase. The volume ratio was 50 ∶ 50 and the flow rate was 0.9 mL/min,when C18(250 mm ×4.6 mm,5.0 μm)was used as separation column,the detection wavelength was 230 nm and the liquid volume was 20 μL. The average recovery of hippuric acid was 96.79 %-98.10 %,the relative standard deviation(RSD)was 0.58 %-1.07 %,the average recovery of benzoic acid was 93.54 %-98.99 %,and RSD was 0.71 %-1.19 %. The established new method has high sensitivity and good reproducibility for qualitative and quantitative analysis.
A rapid method was established for simultaneous determination of hippuric acid and benzoic acid via high performance liquid chromatography. In this experiment,different precipitants,mobile phase,flow rate,recovery rate and minimum detection limit were discussed. The results showed that hippuric acid and benzoic acid ranged of 1 μg/mL-100 μg/mL had strong linearity in the detection and the minimum detection concentration was 0.038 μg/mL when methanol and 0.4 % acetic acid aqueous solution were used as mobile phase. The volume ratio was 50 ∶ 50 and the flow rate was 0.9 mL/min,when C18(250 mm ×4.6 mm,5.0 μm)was used as separation column,the detection wavelength was 230 nm and the liquid volume was 20 μL. The average recovery of hippuric acid was 96.79 %-98.10 %,the relative standard deviation(RSD)was 0.58 %-1.07 %,the average recovery of benzoic acid was 93.54 %-98.99 %,and RSD was 0.71 %-1.19 %. The established new method has high sensitivity and good reproducibility for qualitative and quantitative analysis.
引文
[1]吴丽莉.发酵乳制品中苯甲酸的来源及水平[J].中国乳品工业,2007,35(3):43-46
[2]谢继志.液态乳制品科学与技术[M].北京:中国轻工业出版社,1999:4-32
[3]中华人民共和国卫生部. GB 2760-2014食品安全国家标准食品添加剂使用标准[S].北京:中国标准出版社,2016
[4]李菊,刘淑君,黄雪琳.苯甲酸和苯甲酸钠安全性与检测方法研究进展[J].粮食与油脂,2012(9):49-51
[5]吴春生,李键,骞宇,等.牦牛乳及牦牛酸乳营养价值的研究现状[J].乳业科学与技术,2012,35(3):43-46
[6] NAGAYAMA T, NISHIJIMA M, YASUDA K, et al. Benzoic acid in agricultural food products and processed foods[J]. Journal of the Food Hygienic Society of Japan, 1986, 27(3):316-325
[7]张静,梁颖,张伟,等.毛细管电泳-紫外检测法同时测定人尿中马尿酸和甲基马尿酸[J].分析试验室, 2013(4):118-121
[8]中华人民共和国国家卫生和计划生育委员会. GB 5009.28-2016食品安全国家标准食品中苯甲酸、山梨酸和糖精钠的测定[S].北京:中国标准出版社, 2016
[9] MIHYAR G F, YOUSIF A K, YAMANI M I. Determination of benzoic and sorbic acids in labaneh by high performance liquid chromatography[J]. Journal of Food Composition and Analysis, 1999,12(1):53-61
[10] TOPPINO P M, VOLPATO R, AMELOTTI G. Simultaneous HPLC analysis of sorbic and benzoic acids content in milk products[J].Scienza e Tecnica Lattiero-Casearia, 1990:137-152
[11]张辉,陈美莲.乳与乳制品中山梨酸、苯甲酸的液相色谱检测方法[J].乳业科学与技术, 2005, 27(5):216-217
[12]郭文丽,汪晓东,廖振宇,等.乳制品中马尿酸HPLC的测定[J].食品研究与开发, 2015, 36(6):77-79. DOI:10.3969/j.issn.1005-6521.2015.06.021
[13]冯翠霞,张艳,林丽玲,等.高效液相色谱法测定尿中马尿酸、甲基马尿酸三种同分异构体[J].广东化工, 2010, 37(7):245-246
[14] TARDIF R, BRODEUR J, PLAA G L. Simultaneous high performance liquid chromatographic analysis of hippuric acid and ortho-,meta-,and para-methylhippuric acids in urine[J]. Journal of Analytical Toxicology, 1989, 13(6):313-316
[15]屈莉,杨元.高效液相色谱法直接测定尿中马尿酸[J].职业卫生与病伤, 2013(1):47-49
[16]陈莹蓉,马越鸣,张宁.高效液相色谱法测定大鼠血浆中桂皮酸和马尿酸[J].药物分析杂志, 2009(2):212-216
[17]章唯.红原牦牛乳制品中苯甲酸溯源分析[J].食品界, 2017(7):103-104
[18]赵贞,刘春霞,刘丽君,等.高效液相色谱法检测乳品中的马尿酸和苯甲酸[J].乳业科学与技术, 2017(2):27-29
[19]张强.乳制品中苯甲酸的色谱分析方法研究进展[J].中国奶牛,2017(6):45-48
[20]祝伟霞,魏蔚,杨冀州,等.高效液相色谱法测定乳饮料和奶制品中苯甲酸和山梨酸[J].中国国境卫生检疫杂志,2005,28(5):280-282
[21]王淼,黄晓林.高效液相色谱法同时测定乳及乳制品中防腐剂和甜味剂[J].中国乳品工业,2010,38(11):41-52
[22]谢国祥,吴丽莉,宋如森,等.乳制品中马尿酸的检测及其在发酵过程中动态变化研究[J].食品科学,2005(9):408-411
[2]谢继志.液态乳制品科学与技术[M].北京:中国轻工业出版社,1999:4-32
[3]中华人民共和国卫生部. GB 2760-2014食品安全国家标准食品添加剂使用标准[S].北京:中国标准出版社,2016
[4]李菊,刘淑君,黄雪琳.苯甲酸和苯甲酸钠安全性与检测方法研究进展[J].粮食与油脂,2012(9):49-51
[5]吴春生,李键,骞宇,等.牦牛乳及牦牛酸乳营养价值的研究现状[J].乳业科学与技术,2012,35(3):43-46
[6] NAGAYAMA T, NISHIJIMA M, YASUDA K, et al. Benzoic acid in agricultural food products and processed foods[J]. Journal of the Food Hygienic Society of Japan, 1986, 27(3):316-325
[7]张静,梁颖,张伟,等.毛细管电泳-紫外检测法同时测定人尿中马尿酸和甲基马尿酸[J].分析试验室, 2013(4):118-121
[8]中华人民共和国国家卫生和计划生育委员会. GB 5009.28-2016食品安全国家标准食品中苯甲酸、山梨酸和糖精钠的测定[S].北京:中国标准出版社, 2016
[9] MIHYAR G F, YOUSIF A K, YAMANI M I. Determination of benzoic and sorbic acids in labaneh by high performance liquid chromatography[J]. Journal of Food Composition and Analysis, 1999,12(1):53-61
[10] TOPPINO P M, VOLPATO R, AMELOTTI G. Simultaneous HPLC analysis of sorbic and benzoic acids content in milk products[J].Scienza e Tecnica Lattiero-Casearia, 1990:137-152
[11]张辉,陈美莲.乳与乳制品中山梨酸、苯甲酸的液相色谱检测方法[J].乳业科学与技术, 2005, 27(5):216-217
[12]郭文丽,汪晓东,廖振宇,等.乳制品中马尿酸HPLC的测定[J].食品研究与开发, 2015, 36(6):77-79. DOI:10.3969/j.issn.1005-6521.2015.06.021
[13]冯翠霞,张艳,林丽玲,等.高效液相色谱法测定尿中马尿酸、甲基马尿酸三种同分异构体[J].广东化工, 2010, 37(7):245-246
[14] TARDIF R, BRODEUR J, PLAA G L. Simultaneous high performance liquid chromatographic analysis of hippuric acid and ortho-,meta-,and para-methylhippuric acids in urine[J]. Journal of Analytical Toxicology, 1989, 13(6):313-316
[15]屈莉,杨元.高效液相色谱法直接测定尿中马尿酸[J].职业卫生与病伤, 2013(1):47-49
[16]陈莹蓉,马越鸣,张宁.高效液相色谱法测定大鼠血浆中桂皮酸和马尿酸[J].药物分析杂志, 2009(2):212-216
[17]章唯.红原牦牛乳制品中苯甲酸溯源分析[J].食品界, 2017(7):103-104
[18]赵贞,刘春霞,刘丽君,等.高效液相色谱法检测乳品中的马尿酸和苯甲酸[J].乳业科学与技术, 2017(2):27-29
[19]张强.乳制品中苯甲酸的色谱分析方法研究进展[J].中国奶牛,2017(6):45-48
[20]祝伟霞,魏蔚,杨冀州,等.高效液相色谱法测定乳饮料和奶制品中苯甲酸和山梨酸[J].中国国境卫生检疫杂志,2005,28(5):280-282
[21]王淼,黄晓林.高效液相色谱法同时测定乳及乳制品中防腐剂和甜味剂[J].中国乳品工业,2010,38(11):41-52
[22]谢国祥,吴丽莉,宋如森,等.乳制品中马尿酸的检测及其在发酵过程中动态变化研究[J].食品科学,2005(9):408-411