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    高效液相色谱-示差折光检测器法测定复配消毒液中3种双链季铵盐的含量

    Determination of 3 Double-Chain Quaternary Ammonium Salts in Compound Disinfectant by High Performance Liquid Chromatography Combined with Differential Refractive Index Detector

    • 摘要: 提出了高效液相色谱-示差折光检测器法测定复配消毒液中二癸基二甲基氯化铵、辛基癸基二甲基氯化铵、二辛基二甲基氯化铵等3种双链季铵盐含量的方法。复配消毒液样品经流动相稀释,以Welchrom C18色谱柱为固定相,以体积比70∶30的乙腈-0.01 mol·L-1丁烷磺酸钠溶液的混合溶液(pH 3.5)为流动相进行洗脱,采用示差折光检测器测定3种双链季铵盐的含量。结果表明:3种双链季铵盐的质量浓度在50~1 000 mg·L-1内与对应的峰面积呈线性关系,检出限(3S/N)为3.3~5.1 mg·L-1;对实际样品进行3个浓度水平的加标回收试验,回收率为91.0%~105%,测定值的相对标准偏差(n=6)为1.3%~2.2%。采用独立样本t检验法比对本方法与高效液相色谱-蒸发光散射检测器法是否具有显著性差异,结果显示两组检测结果t值为1.85,P值为0.089,表明无显著性差异。

       

      Abstract: A method for the determination of 3 double-chain quaternary ammonium salts, including didecyl dimethyl ammonium chloride, octyldecyl dimethyl ammonium chloride, dioctyldimethyl ammonium chloride in compound disinfectant by high performance liquid chromatography combined with differential refractive index detector was proposed. The compound disinfectant sample was diluted by the mobile phase and eluted by Welchrom C18 column as the stationary phase, and the mixed solution (pH 3.5) composed of acetonitrile and 0.01 mol·L-1 sodium butane sulfonate solution at volume ratio of 70\:30 as the mobile phase. It was shown that linear relationships between the mass concentrations and corresponding peak areas of 3 double-chain quaternary ammonium salts were found in the range of 50-1 000 mg·L-1, with detection limits (3S/N) in the range of 3.3-5.1 mg·L-1. Test for recovery was made on the actual sample at 3 concentration levels by standard addition method, giving results in the range of 91.0%-105%, with RSDs (n=6) of the determined values in the range of 1.3%-2.2%. The independent sample t-test was used to compare whether there was significant difference between the proposed method and high performance liquid chromatography combined with evaporative light scattering detector. It was shown that t value and P value of the detection results of the two groups were 1.85 and 0.089, respectively, indicating there was no significant difference.

       

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