昆明市售卫生纸中11种荧光增白剂监测结果分析

目的 为了解昆明市售卫生纸中11种荧光增白剂的添加情况。方法 样品采集自昆明市超市销售的60份不同品牌卫生纸, 粉碎后经用40%乙腈-水超声提取3次, 合并提取液, 离心, 上清液经正己烷脱脂。脱脂后的溶液用高效液相色谱法检测, 外标法定量。结果 本方法在17 min内完成11种目标化合物的分离分析, 线性关系良好, 相关系数(R2)均大于0.99。在低、中和高3个添加水平的回收率为84.2%~99.8%, 相对标准偏差(relative standard deviations, RSDs)小于5.2%(n=6), 方法定量限(limits of quantitation, LOQ)为2.4~3.8 mg/kg, 各品牌卫生纸中, 阳性样品检出率达到8.33%, 含量最高达10.5 mg/kg。结论 昆明市售卫生纸中存在添加荧光增白剂, 部分样品中检测出多种荧光增白剂非法添加, 相关部门应该予以重视, 加强对市售卫生纸的监督管理。

Analysis of monitoring results of 11 fluorescent whitening agents in toilet tissue sold in Kunming

Objective To evaluate the addition of 11 fluorescent whitening agents in toilet paper sold in Kunming. Methods The 60 different brands toilt tissues were collected from the market in Kunming. The crushed samples were extracted by 40% acetonitrile-water for 3 times, combined with the extract and centrifugated. Then the supernatant was degreased by n-hexane. After degreasing, the solution was determined by high performance liquid chromatography. The external standard method was used. Results The separation and analysis of 11 target compounds were achieved within 17 min, and the correlation coefficients (R2) were more than 0.99. The recoveries were ranged from 84.2% to 99.8% for 11 kinds of fluorescent whitening agents with 3 spiked levels of low, middle and high concentrations. The relative standard deviations (RSDs) were less than 5.2% (n=6), and the limits of quantitation (LOQ) for the 11 kinds of fluorescent whitening agents were 2.4~3.8 mg/kg. The detection rate of positive samples reached 8.33% and the highest content was 10.5 mg/kg. Conclusion Fluorescent whitening agents still exist in toilt tissues in Kunming, and a variety of fluorescent whitening agents illegally added in some samples are detected. The relevant supervision should pay more attention and strengthen the monitoring of toilt tissues.