分光光度法和高效液相色谱法测定啤酒中残留直链烷基苯磺酸钠含量  

Determination of linear alkylbenzene sulfonate residues in beer by spectrophotometry and high performance liquid chromatography

作　　者：李旭 周蓉 LI Xu;ZHOU Rong(Jingmen Food and Drug Quality Inspection Institute,Jingmen 448124,China;Shayang County Public Inspection and Testing Center,Shayang 448200,China)

机构地区：[1]荆门市食品药品质量检验所,荆门448124 [2]沙洋县公共检验检测中心,沙洋448200

出　　处：《食品安全质量检测学报》2020年第5期1616-1625,共10页Journal of Food Safety and Quality

摘　　要：目的建立分光光度法和高效液相色谱法测定啤酒中残留直链烷基苯磺酸钠的分析方法。方法确定实验过程主要参数。制作吸光度浓度工作曲线,定量样品检测结果。采用液液萃取法提取样品中的直链烷基苯磺酸钠,在最佳色谱条件下,制作了阴离子表面活性剂(以十二烷基苯磺酸钠计)标准曲线,采用峰高外标法定量样品检测结果。结果通过实验验证亚甲蓝活性物质(methylene-blue active substances,MBAS)的特征吸收波长为652 nm,表观摩尔吸光系数ε=1.93×106 L/(mol·cm),检出限为4.04×10^-3mg/L,检测方法回收率73.4%~104.5%,相对标准偏差3.04%,线性范围为4.04×10^-3~2.0 mg/L。在确定的最佳实验条件下检测了6份啤酒样品,其中直链烷基苯磺酸钠残留量在0.024~0.036 mg/L之间。高效液相色谱法的线性范围是2.0~200 mg/L,检出限为2.05×10^-3 mg/L,回收率为78.6%~98.5%,相对标准偏差≤8.9%。在确定的最佳色谱条件下检测了6个样品,测得啤酒中直链烷基苯磺酸钠的残留量在0.014~0.022 mg/L之间。结论液液萃取高效液相色谱法检测结果的准确度略高于分光光度法,但不宜在低浓度(<2 mg/L)下作标准曲线。对啤酒中残留直链烷基苯磺酸钠的直接快速检测宜选取分光光度法,而准确检测则优先选用液液萃取高效液相色谱法。Objective To establish a method of determination of the linear alkylbenzene sulfonate residues in beer by spectrophotometry and high performance liquid chromatography.Methods Determine the main parameters of experimental process.Making absorbance concentration working curve,Quantitative sample test results.The linear alkylbenzene sulfonate was extracted from samples by liquid liquid extraction.Under the best chromatographic conditions,the standard curve of anionic surfactants(based on sodium dodecylbenzene sulfonate)was made.By using the base high external standard method quantitative sample test results.Results Through the experiment,the methylene blue active substances(MBAS)features absorption wavelength was 652 nm.The apparent molar absorption coefficient wasε=1.93×106 L/(mol cm),the detection limit was 4.04×10^-3 mg/L,the recovery of test method was 73.4%-104.5%,the relative standard deviation was 3.04%,and the linear range was 4.04×10^-3-2.0 mg/L.Six beer samples were tested under the optimum best experimental conditions,among which the residue of the linear alkylbenzene sulfonate was 0.024-0.036 mg/L.The linear range of HPLC was 2.0-200 mg/L,the detection limit was2.05×10^-3 mg/L.The recovery was 78.6%-98.5%,and the relative standard deviation was less than or equal to 8.9%.Six samples were detected under the optimum conditions of chromatographic,the results showed that the residues of the linear alkylbenzene sulfonate in beer were 0.014-0.022 mg/L.Conclusion The accuracy of HPLC is slightly higher than that of spectrophotometry.But it is not suitable to make standard curve at low concentrations(<2 mg/L).Spectrophtometry could be selected for the direct and rapid testing of the residual sodium linear alkylbenzene sulfonate in beer,and LLE-HPLC could be preferred for the accurate detection.

关 键 词：啤酒 直链烷基苯磺酸钠 分光光度法 高效液相色谱法 

分 类 号：O657[理学—分析化学] TS262.5[理学—化学]