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    高效液相色谱法同时测定纺织品中11种二苯甲酮类紫外吸收剂

    Simultaneous Determination of 11 Benzophenone-Type Ultraviolet Absorbents in Textiles by HPLC

    • 摘要: 剪碎后的纺织品样品0.500 0 g经30 mL甲醇于60 ℃超声提取30 min,冷却至室温后,取上清液用0.45 μm有机滤膜过滤,采用高效液相色谱法同时测定滤液中11种二苯甲酮类紫外吸收剂的含量。以xBridge shield RP C18色谱柱(250 mm×4.6 mm,5 μm)为分离柱,用0.1%(体积分数,下同)甲酸溶液和含0.1%甲酸的甲醇-异丙醇溶液(甲醇与异丙醇体积比为7:3)以不同比例混合的溶液为流动相进行梯度洗脱,在检测波长280 nm处进行测定。11种二苯甲酮类紫外吸收剂的质量浓度均在0.5~20.0 mg·L-1内与其对应的峰面积呈线性关系,检出限(3S/N)为3~9 mg·kg-1,测定下限(10S/N)为9~27 mg·kg-1。以空白样品为基体进行加标回收试验,所得回收率为87.6%~107%,测定值的相对标准偏差(n=6)为1.9%~8.3%。方法应用于33批次的防紫外线纺织产品样品的分析,4-羟基二苯甲酮在所有样品中均未检出,其他二苯甲酮类紫外吸收剂均在样品中有不同程度的检出,2-羟基-4-甲氧基二苯甲酮的检出率最高,达到了58%,质量分数在42~261 mg·kg-1之间。

       

      Abstract: The shredded textile sample (0.500 0 g) was extracted ultrasonically at 60 ℃ for 30 min with 30 mL of methanol. After cooling to room temperature,the supernatant was taken and filtered with 0.45 μ m organic filter membrane. HPLC was applied to the simultaneous determination of 11 benzophenone-type ultraviolet absorbents in the filtrate. xBridge shield RP C18 chromatographic column (250 mm×4.6 mm, 5 μm) was used as separation column, and mixtures of 0.1% (φ, the same below) formic acid solution and methanol-isopropanol solution (volume ratio of 7∶3) containing 0.1% formic acid with different mixing ratios were used as mobile phase in the gradient elution. Detection at 280 nm was adopted in the determination. Linear relationships between values of peak area and mass concentration of the 11 benzophenone-type ultraviolet absorbents were kept in the same range of 0.5-20.0 mg·L-1, with detection limits (3S/N) in the range of 3-9 mg·kg-1 and lower limits of determination (10S/N) in the range of 9-27 mg·kg-1. On the base of blank sample, test for recovery was made by standard addition method; values of recovery found were in the range of 87.6%-107%, with RSDs (n=6) of determined values in the range of 1.9%-8.3%. The method was used to analyze samples of 33 batches of anti-ultraviolet fabric. Except that 4-hydroxybenzophenone was not detected in all fabrics, other benzophenone-type ultraviolet absorbents were found in these samples. The highest detection rate of 2-hydroxy-4-methoxybenzophenone was 58%, and the mass fraction of 2-hydroxy-4-methoxybenzophenone was in the range of 42-261 mg·kg-1.

       

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