超声萃取高效液相色谱法测定指画颜料中的6种防腐剂

Determination of Six Preservatives in Finger Paints by Ultrasonic Extraction-High Performance Liquid Chromatography

建立指画颜料中2- 甲基-4- 异噻唑啉-3- 酮、苯甲酸等6 种防腐剂的超声萃取– 高效液相色谱的测定方法。经试验确定，萃取溶剂为100% 甲醇，萃取时间为10 min，萃取温度为25℃。采用Hypersil ODS 柱(250 mm×4.6mm，5 μm)，以乙腈– 水为流动相梯度洗脱，流速为1.0 mL／min，检测波长为245 nm。在0.5~20 mg／L 检测范围内6 种防腐剂的质量浓度与其色谱峰面积呈良好的线性关系，线性相关系数r ≥ 0.999 2，方法检出限为1.15~1.71 μg／L，测定结果的相对标准偏差为1.54%～3.18%(n=8)，加标回收率为84.2%～108.0%。该方法操作简单，灵敏度高，可用于指画颜料中6 种防腐剂含量的分析检测。

A method for determination of six preservatives compounds such as 2-methyl-4-isothiazolin-3-one, benzoic acid, etc. in finger paints by ultrasonic extraction–high performance liquid chromatography was developed. The extraction solvent was 100% methanol,extraction time was 10 min and extraction temperature was 25℃ . The chromatographic separation was carried out on Hypersil ODS column (250 mm×4.6 mm,5 μm). Mobile phase was acetonitrile–water for gradient elution with flow rate of 1.0 mL/min. The wavelength of UV for the HPLC detection was set at 245 nm. The consentration of six preservatives was linear with its chromatographic peak area in the detection range of 0.5–20 mg/L, the correlation coefficent was not less than 0.999 2. The detection limit of the method was 1.15–1.71 μg/L, the relative standard deviation of detection results was 1.54%–3.18%(n=8), the addition recoveries were 84.2%–108.0%. The method is simple to operate with higher sensitivity, it is suitable for the determination of six preservatives in finger paints.