摘要
提出了高效液相色谱法测定造型黏土中2种防腐剂(2-甲基-4-异噻唑啉-3-酮和5-氯-2-甲基-4-异噻唑啉-3-酮)的方法。黏土样品以甲醇进行超声提取,所得提取液以柱温为35℃的Agilent Eclipse XDB-C18色谱柱为分离柱,用甲醇与水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275nm处进行测定。2种防腐剂的质量浓度均在0.50~40mg·L-1范围内与其峰面积呈线性关系,检出限(3S/N)分别为6.80,14.8μg·L-1。方法用于造型黏土样品分析,加标回收率在90.9%~120%之间,测定值的相对标准偏差(n=6)在0.060%~2.4%之间。
A method of HPLC for the determination of 2 preservatives (i. e. , 2-methyl-4-isothiazolin-3-on and 5-chloro-2-methyl-4-isothiazolin-3-one) in moulding clay was proposed. The sample was extracted ultrasonically with methanol. The extract was separated by chromatography by using Agilent Eclipse XDB C18 column (at column temp. of 35 ℃) as separation column, and mixtures of methanol and water in various ratios as mobile phase in gradient elution- UV-detection at 275 nm was adopted in the determination. Linear relationships between values of peak area and mass concentration of the 2 preservatives were kept in the same range of 0. 50-40 mg · L-1 , with detection limits (3S/N) of 6. 80, 14. 8 μg · L-1 respectively. The proposed method was applied to the analysis of substantial samples. Values of recovery found by standard addition method were in the range of 90. 9o/oo- 120%, and RSD's (n=6) found were in the range of 0. 060%-2.4%.
出处
《理化检验(化学分册)》
CAS
CSCD
北大核心
2016年第2期171-175,共5页
Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
基金
国家质检总局风险监测任务(监测中心[2015]7号)