水浸提-乙醚提取-碱溶液反提取-高效液相色谱法测定多种基质食品中丙酸的含量  

Determination of Propionic Acid in Foods with Multiple Matrices by High Performance Liquid Chromatography with Water Leaching,Ether Extraction and Alkali Solution Reverse Extraction

作　　者：章再婷 曹苏仙 葛晓鸣 刘忠义 陈颖 方科益 ZHANG Zaiting;CAO Suxian;GE Xiaoming;LIU Zhongyi;CHEN Ying;FANG Keyi(Ningbo Joysun Product Testing Company,Ningbo 315040,China;Technology Center of Ningbo Customs,Ningbo 315040,China)

机构地区：[1]宁波中盛产品检测有限公司,宁波315040 [2]宁波海关技术中心,宁波315040

出　　处：《理化检验（化学分册）》2024年第10期1000-1003,共4页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

摘　　要：鉴于现有检测食品中丙酸的前处理方法存在基质净化效果差、耗费时间长等缺点,进行了题示研究。取5 g样品,加入30 mL水,涡旋5 min,超声30 min。冷却至室温后,将溶液酸度调节至p H7.0±0.5,加入183 g·L^(-1)乙酸锌溶液和92 g·L^(-1)亚铁氰化钾溶液各0.6 mL,用水稀释至50 mL,混匀,离心5 min。取1.0 mL上清液,加入1 mol·L^(-1)磷酸溶液40μL和2.5 mL乙醚,涡旋5 min,离心5 min。重复提取过程一次,合并乙醚层,加入0.025 mol·L^(-1)氢氧化钠溶液1.0 mL,涡旋5 min,离心5 min。收集下层相,过0.45μm尼龙滤膜。滤液进入高效液相色谱仪,在Thermo Hypersil Gold C18色谱柱上以体积比5∶95的甲醇和1.5 g·L^(-1)磷酸氢二铵溶液的混合溶液(p H 2.6,用磷酸调节)为流动相等度洗脱分离丙酸,在214 nm波长下测定。结果显示:丙酸的质量浓度在0.01~0.5 g·L^(-1)内和峰面积呈线性关系,检出限(3S/N)为0.03 g·kg^(-1)。对多种基体食品进行3个浓度水平的加标回收试验,回收率为84.8%~95.3%,测定值的相对标准偏差(n=6)为2.8%~6.2%。方法用于多基质食品的分析,检测结果与GB 5009.120—2016中蒸馏法的相对误差绝对值不大于10%。In view of the shortcomings of poor matrix purification effect and long time consumption in the existing pretreatment methods for detecting propionic acid in food,the research mentioned by the title was conducted.An aliquot(5 g)of sample was taken,and 30 mL of water was added.The mixture was vortexed for 5 min,and sonicated for 30 min.After cooling to room temperature,the acidity of the solution was adjusted to pH 7.0±0.5.The 0.6 mL of 183 g·L^(−1) zinc acetate solution and 0.6 mL of 92 g·L^(−1) potassium ferrocyanide solution were added,and the solution obtained was diluted to 50 mL by water.After mixing evenly and centrifuging for 5 min,1.0 mL of supernatant was taken,and 40μL of 1 mol·L^(−1) phosphoric acid solution and 2.5 mL of ether were added.The mixed solution was vortexed for 5 min,and centrifuged for 5 min.The extraction process was repeated once,and the ether layers were combined.Then 1.0 mL of 0.025 mol·L^(−1) sodium hydroxide solution was added,and the mixed solution was vortexed for 5 min,and centrifuged for 5 min.The lower phase was collected,and passed through a 0.45μm nylon filter membrane.The filtrate was introduced into the high performance liquid chromatograph,and propionic acid was separated by gradient elution with a mixture(pH 2.6,adjusted by phosphoric acid)of methanol and 1.5 g·L^(−1) diammonium hydrogen phosphate solution at volume ratio of 5∶95 as the mobile phase on Thermo Hypersil Gold C18 column,and determined at wavelength of 214 nm.It was shown that linear relationship between values of the mass concentration and peak area of propionic acid was kept in the range of 0.01-0.5 g·L^(−1),with detection limit(3S/N)of 0.03 g·kg^(−1).Test for recovery was made at the 3 concentration levels on foods with multiple matrices by standard addition method,giving recoveries in the range of 84.8%-95.3%and RSDs(n=6)in the range of 2.8%-6.2%.The proposed method was used for the analysis of foods with multiple matrices,and absolute values of relative errors between detection

关 键 词：食品 丙酸 高效液相色谱法 水直接浸提法 反提取 

分 类 号：O657.7[理学—分析化学]