高效液相色谱法直接测定洗衣粉中直链烷基苯磺酸钠
Direct HPLC Determination of n-Alkyl Benzene Sulfonates in Powder Detergent
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摘要: 提出了用反相高效液相色谱法测定洗衣粉中直链烷基苯磺酸钠(n-ABS).研究并选定方法的最佳分析条件为:① 固定相为Venusil XBP-C18(4.6 mm×250 mm,5 μm)色谱柱;② 流动相由乙腈和0.1 mol·L-1 NaClO4水溶液以6比4混合的溶液;③ 流动相的流速为1.0 mL·min-1;④ 柱温40 ℃;⑤ 紫外检测波长为225 nm.按上述分析条件进行测定,不仅可达到n-ABS同系物之间的良好分离并测得样品的平均碳数和平均相对分子质量,而且与同分异构体也能得到较好分离,按所提出的方法,可在22 min以内完成一次分析.标准曲线的回归方程为y=7 552.4 x-5 282.3,相关系数为0.999 6.方法的检出限(3S/N)为1.0 mg·L-1,相对标准偏差(n=6)为0.3%,回收率在96.3%~105.0%之间.Abstract: A reversed phase HPLC method for determination of sodium n-alkyl benzene sulfonates (n-ABS) in powder detergent was proposed.Analytical conditions of the method were studied and the optimum conditions found were as follows: ① stationary phase: Venusil XBP-C18 (4.6 mm×250 mm,5 μm) chromatographic column;② mobile phase: a mixed solution of acetonitrile and aq.solution of 0.1 mol·L-1 NaClO4,mixed in the ratio of 6 to 4 by vol.;③ flow-rate of mobile phase: 1.0 mL·min-1;④ column temperature: 40 ℃;⑤ wavelength for UV-detection: 225 nm.By applying the conditions given above,homologues of n-ABS were very well separated and the average number of carbon atom and the average relative molecular mass of the sample were found;and in addition,isomers of n-ABS were also separated.By the proposed method,analysis of a sample was completed within 22 min.Linear regression equation of the standard curve was found as follows: y=7 552.4 x-5 282.3 (r=0.999 6),and detection limit (3S/N) found was 1 mg·L-1.Precision and recovery of the method were tested,and values of RSD (n=6) and recovery found were 0.3% and in the range of 96.3%-105.0%.