摘要
优化纺织品中(甲基)丙烯酸类化合物的前处理及仪器条件,建立同步测定纺织品中(甲基)丙烯酸类化合物的HPLC-MS分析方法。前处理以甲醇为萃取试剂,优化条件为:萃取体积10 mL、萃取温度50℃、萃取时间40 min、超声功率450 W。色谱条件采用ZORBAX EclipsePlusC18色谱柱,流速0.1 mL/min;流动相为水与甲醇(体积比为95∶5),并用氨水调节pH至9.8。结果表明:丙烯酸的检出限(LOD)为1.80 mg/kg,定量限(LOQ)为5.30 mg/kg;甲基丙烯酸的LOD为0.77 mg/kg,LOQ为2.40 mg/kg。在0.50~100.00 mg/L质量浓度范围内,线性关系良好(R^(2)≥0.9993);低、中、高3个质量分数(5、500、1000 mg/kg)加标回收率≥81.74%,相对标准偏差(RSD)≤2.89%。方法灵敏度、准确度和精密度良好。
The pretreatment and instrumental conditions for(methyl)acrylic acid compounds in textiles were optimized,and an HPLC-MS analytical method for the simultaneous determination of(methyl)acrylic acid compounds in textiles was developed.For pretreatment,methanol was used as the extraction solvent,with optimized parameters including:extraction volume of 10 mL,extraction temperature of 50℃,extrac⁃tion time of 40 min,and ultrasonic power of 450 W.The chromatographic conditions were as follows:a ZOR⁃BAX Eclipse Plus C18 column was employed,with a flow rate of 0.1 mL/min;the mobile phase consisted of water-methanol(95∶5,volume ratio),and the pH was adjusted to 9.8 using ammonia solution.Results indi⁃cated that:the limit of detection(LOD)of acrylic acid was 1.80 mg/kg,and the limit of quantification(LOQ)was 5.30 mg/kg;for methacrylic acid,the LOD was 0.77 mg/kg,and the LOQ was 2.40 mg/kg.Within the mass concentration range of 0.50-100.00 mg/L,the method exhibited good linearity(R^(2)≥0.9993).For spiked recovery tests at three mass fractions(low:5 mg/kg,medium:500 mg/kg,high:1000 mg/kg),the re⁃covery rates were≥81.74%,and the relative standard deviations(RSD)were≤2.89%.The method demon⁃strated good sensitivity,accuracy,and precision.
作者
赵海浪
刘宇
徐红
ZHAO Hailang;LIU Yu;XU Hong(Shanghai Institute of Quality Inspection and Technical Research Co.,Ltd.,Shanghai 200040,China;Key Laboratory of the Ministry of Eco-Textile Education,Donghua University,Shanghai 201620,China)
出处
《纺织检测与标准》
2025年第4期1-5,共5页
Textile Testing and Standard
基金
上海市市场监督管理局科技项目(2024-27)。
关键词
丙烯酸
甲基丙烯酸
高效液相色谱-质谱法
acrylic acid
methacrylic acid
high-performance liquid chromatography-mass spectrometry
