Food and Fermentation Industries >

2021 , Vol. 47 >Issue 14: 257 - 263

DOI: https://doi.org/10.13995/j.cnki.11-1802/ts.026494

Determination of propionic acid and its salts in cakes by liquid-liquid extraction-GC-MS combined with dual enzymatic hydrolysis

  • WANG Yu ,
  • ZHONG Yuxin ,
  • CHEN Yueming ,
  • HUANG Jingchu ,
  • CHEN Sui ,
  • SU Yanyu ,
  • CHEN Jiaxin ,
  • CAI Weiyi
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  • 1(Guangzhou Institute for Food Inspection,Guangzhou 511400,China)
    2(Guangdong Meiweixian Flavoring Foods Co.Ltd.,Zhongshan 528437,China)

Received date: 2020-12-17

  Revised date: 2021-02-02

  Online published: 2021-08-20

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Abstract

A gas chromatography-mass spectrometry using liquid-liquid extraction combined with dual enzymatic hydrolysis for determination of propionic acid in cakes was developed successfully.The sample was hydrolyzed in phosphate buffer at 37 ℃ to remove protein and starch.Propionic acid was converted to ionic state while the pH of hydrolyzed solution was adjusted to pH>10.Non-polar impurities were removed by ether extraction.Propionic acid was converted to molecular state by adjusting the aqueous phase pH<4. The propionic acid was extracted by ethyl acetate in order to remove polar impurities.The target analyte were separated on DB-WAX capillary column (30 m×0.25 mm,0.25 μm),and detected by gas chromatography-mass spectrometry.The results indicated that the calibration curve for propionic acid was linear in the range of 0.1-20 μg/mL with the correlation coefficient of 1.000.The spike recoveries were 83%-109%,RSD<7%.The detection limit was 0.450 mg/kg.The developed method has the advantages of simple pretreatment,high sensitivity,accuracy and fast.

Key words： propionic acid; gas chromatography and mass spectrometry (GC-MS); enzymatic hydrolysis; degreasing; pastries; pH

Cite this article

WANG Yu , ZHONG Yuxin , CHEN Yueming , HUANG Jingchu , CHEN Sui , SU Yanyu , CHEN Jiaxin , CAI Weiyi . Determination of propionic acid and its salts in cakes by liquid-liquid extraction-GC-MS combined with dual enzymatic hydrolysis[J]. Food and Fermentation Industries, 2021 , 47(14) : 257 -263 . DOI: 10.13995/j.cnki.11-1802/ts.026494

References

[1] 闫克玉, 王岁楼.新型食品添加剂丙酸锌的制备及应用性能研究[J].食品与发酵工业,2002,28(6):1-4.
YAN K Y,WANG S L,et al.Preparation and application of zinc propionate as a new food additive[J].Food and Fermentation Industries,2002,28(6):1-4.
[2] 徐虹, 欧阳平凯,王莎莎.发酵法生产丙酸[J].食品与发酵工业,1997,23(6):62-65.
XU H,OUYANG P K,WANG S S,et al.Production of propionic acid by fermentation[J].Food and Fermentation Industries,1997,23(6):62-65.
[3] 中华人民共和国国家质量监督检验检疫局, 中国国家标准化管理委员会.GB/T 20997—2007 糕点通则[S].北京:中国标准出版社,2007.
State Administration of Quality Supervision,Inspection and Quarantine of the People's Republic of China,China National Standardization Administration Committee.GB/T 20997—2007 General technical requirement for the pastry[S].Beijing:Standards Press of China,2007.
[4] 王瑞, 何涛.食品中的丙酸本底含量及产生机理研究进展[J].中国调味品,2015,40(9):104-106.
WANG R,HE T.Research progress of the intrinsic content of propionic acid in food and its generation mechanism[J].China Condiment,2015,40(9):104-106.
[5] 中华人民共和国国家卫生和计划生育委员会.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,2014.
State Health and Family Planning Commission of the People's Republic of China.GB 2760—2014 National food safety standard for uses of food additives[S].Beijing:Standards Press of China,2014.
[6] 瞿春芳.直接浸提-气相色谱法测定食品中的丙酸钙[J].化学分析计量,2011,20(5):58-59.
QU C F.Determination of calcium propionate in food by direct extraction-gas chromatography[J].Chemical Analysis and Meterage,2011,20(5):58-59.
[7] 李歆, 林桢,杨芳,等.水蒸馏提取-离子色谱法检测酱油中丙酸钙[J].食品科技,2013,38(5):339-341.
LI X,LIN Z,YANG F,et al.Steam distillation extraction-ion chromatography with conductivity detection for the determination of calcium propionate in soy sauce[J].Food Science and Technology,2013,38(5):339-341.
[8] 李霞, 刘旭,李玲,等.气相色谱测定食品中丙酸及其盐类[J].色谱,2019,37(2):227-232.
LI X,LIU X,LI L,et al.Determination of propionic acid and its salts in food by gas chromatography[J].Chinese Journal of Chromatography,2019,37(2):227-232.
[9] 闫肃. 强阴离子交换柱法测定蛋糕中丙酸钙(钠)[J].广州化工,2015,43(15):102-104.
YAN S.Calcium (sodium) propionate in cakes measured by strong anion-exchange column[J].Guangzhou Chemical Industry,2015,43(15):102-104.
[10] 邹沫君. RP-HPLC法测面包中丙酸[J].食品工业,2020,41(1):288-290.
ZOU M J.Determination of the propanoic acid in bread by RP-HPLC[J].The Food Industry,2020,41(1):288-290.
[11] 熊建军, 邹大维,杨坤,等.离子色谱法检测月饼中丙酸及其盐类分析研究[J].现代食品,2018,12:98-101.
XIONG J J,ZOU D W,YANG K,et al.Determination of propionic acid and its salts in moon cakes by ion chromatography[J].Modern Food,2018,12:98-101.
[12] 卢兰香, 孙珊珊,薛霞,等.高效液相法测定食品中丙酸及盐类[J].食品工业科技,2019,40(11):234-240.
LU L X,SUN S S,XUE X,et al.Determination of propionic acid and its salts in food by high performance liquid chromatography[J].Science and Technology of Food Industry,2019,40(11):234-240.
[13] 王峰. 糕点中丙酸盐的气液相色谱分析方法比较[J].食品与发酵科技,2014,50(4):61-63.
WANG F.The comparison of gas chromatography and liquid chromatography analysis methods for propionate in pastry[J].Food and Fermentation Technology,2014,50(4):61-63.
[14] 高海军, 范自营,张红云,等.气相色谱法同时快速测定食品中丙酸、山梨酸、苯甲酸及脱氢乙酸[J].粮油食品科技,2017,5(25):47-51.
GAO H J,FAN Z Y,ZHANG H Y,et al.Simultaneous and rapid determination of propionic acid,sorbic acid,benzoic acid and dehydroacetic acid in food by gas chromatography[J].Science and Technology of Cereals,Oils and Foods,2017,5(25):47-51.
[15] 国家卫生和计划生育委员会.GB 5009.120—2016 食品中丙酸钠、丙酸钙的测定[S].北京:中国标准出版社,2016.
National Health and Family Planning Commission.GB 5009.120—2016 Determination of sodium propionate and calcium propionate in food[S].Beijing:Standards Press of China,2016.
[16] AZZAM K M A,SAAD B,HASHIM N H,et al.Determination of propionates and propionic acid in bakery products using gas chromatography[J].International Food Research Journal,2010,17(4):1 107-1 112.
[17] 焦阳,郑鹏宇,于兵,等.气相色谱-质谱法测定酱菜中的丙酸残留[J].检验检疫学刊,2012,22(1):13-16.
JIAO Y,ZHENG P Y,YU B,et al.Determination of propionic acid residue in soy sauce pickles using GC-MS[J].Journal of Inspection and Quarantine,2012,22(1):13-16.
[18] 郝鹏飞,刘东风,牟志春,等.气相色谱-质谱法测定腌渍蔬菜中的丙酸及其应用[J].食品研究与开发,2013,34(23):98-100.
HAO P F,LIU D F,MU Z C,et al.Determination and application of propionic acid in pickled vegetables by GC-MS[J].Food Research and Development,2013,34(23):98-100.
[19] 刘雪莲, 申培立,牛丹丹,等.地衣芽胞杆菌α-淀粉酶耐热耐酸突变体的酶学性质[J].食品与发酵工业,2020,46(2):7-10.
LIU X L,SHEN P L,NIU D D,et al.Biochemical sharacterization of heat and acid-resistant mutant of Bacillus licheniform is α-amylase[J].Food and Fermentation Industries,2020,46(2):7-10.
[20] 马银凤, 申培立,王彩喆,等.中温α-淀粉酶的分子进化及酶学性质[J].食品与发酵工业,2021,47(11):14-18.
MA Y F,SHEN P L,WANG C Z,et al.Molecular evolution and biochemical characterization of bacillus amyloliquefaciens α-amylase[J/OL].Food and Fermentation Industries,2021,47(11):14-18.
[21] 韩晔华, 张艳芬,刘虎威.色谱质谱技术在食品安全分析检测中的应用[J].食品安全质量检测学报,2016,7(4):1 578-1 586.
HAN Y H,ZHANG Y F,LIU H W.Application of chromatography and mass spectrometry in food safety analysis[J].Journal of Food Safety and Quality,2016,7(4):1 578-1 586.
[22] 贺燕,徐文泱,孙桂芳,等.气相色谱-质谱法检测肉制品中的杀鼠酮[J].食品与机械,2017,33(5):99-102;124.
HE Y,XU W Y,SUN G F,et al.Determination of pindone in meat product by GC-MS[J].Food & Machinery,2017,33(5):99-102;124.
[23] 姜云鹏.用pH玻璃电极研究丙酸在甲酸-水介质中的热力学性质[J].丹东纺专学报,2003,2(1):5-6.
JIANG Y P.Studying the thermodynamics nature of propionic acid in the mixture of methanol and water solution with pH glass electrode[J].Journal of Dandong Textile College,2003,2(1):5-6.
[24] 赵爱华.乙醚试剂对丙戊酸钠含量测定的影响[J].首都医药,1998,5(3):15.
ZHAO A H.The influence of ether reagent on the determination of sodium valporate[J].Capital Medicine,1998,5(3):15.
[25] 袁焜,刘艳芝,王鹏.非羧酸类有机化合物及其酸性[J].化学教育(中英文),2019,40(2):31-35.
YUAN K,LIU Y Z,WANG P.Non-carboxylic acid organic compounds and their acidity[J].Chinese Journal of Chemical Education,2019,40(2):31-35.
[26] COMMISSION D.Implementing council directive 96/23/EC concerning the performance of analytical methods and the interpretation of results[Z].Official Journal of European Communities,2002/657/EC,L 221/8-27.
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