Determination of Iodopropynyl Butylcarbamate and Zinc Pyrithione in Water-Borne Coating by High Performance Liquid Chromatography
摘 要
取涂料样品约2 g,用10 mL N,N-二甲基甲酰胺(DMF)超声萃取10 min,冷却至室温,离心5 min,取上清液至50 mL容量瓶中。残余物用10 mL乙腈超声萃取10 min,离心5 min,重复2次,合并上清液,用乙腈定容至50 mL。所得溶液经0.22 μm亲水聚四氟乙烯(PTFE)滤膜过滤,在Agilent ZORBAX Eclipse Plus C18柱上进行分离,以体积比7∶3的乙腈-[10 mmol·L-1磷酸二氢钾-1.0 mmol·L-1乙二胺四乙酸二钠(Na2EDTA)溶液(pH 4.0)]混合液为流动相进行等度洗脱,采用高效液相色谱法(HPLC)测定其中碘丙炔醇丁基氨甲酸酯(IPBC)和吡啶硫酮锌(ZPT)的含量,检测波长为235 nm。结果表明,IPBC和ZPT标准曲线的线性范围分别为20~2 000 mg·L-1和50~800 mg·L-1,检出限(3S/N)分别为106,298 mg·kg-1。按照标准加入法进行回收试验,回收率为92.4%~103%,测定值的相对标准偏差(n=6)均小于3.0%。方法用于4种实际样品的分析,仅一种室内用水性涂料检出ZPT,检出量为920 mg·kg-1。
Abstract
The coating sample (about 2 g) was taken, ultrasonically extracted with 10 mL of N,N-dimethylformamide (DMF) for 10 min, cooled to room temperature, and centrifuged for 5 min. The supernatant was taken to a 50 mL-volumetric flask. The residue was ultrasonically extracted with 10 mL of acetonitrile for 10 min, and centrifuged for 5 min. After repeated twice, the supernatants were combined, and made its volume up to 50 mL with acetonitrile. The obtained solution was passed through 0.22 μm hydrophilic polytetrafluoroethylene (PTFE) filtration membrane, and separated on Agilent ZORBAX Eclipse Plus C18 column, using a mixture of acetonitrile and 10 mmol·L-1 potassium dihydrogen phosphate-1.0 mmol·L-1 Na2EDTA solution (pH 4.0) at a volume ratio of 7:3 as the mobile phase for isocratic elution. Iodopropynyl butylcarbamate (IPBC) and zinc pyrithione (ZPT) were determined by high performance liquid chromatography (HPLC), with detection wavelength of 235 nm. As shown by the results, linear ranges of the IPBC and ZPT standard curves were 20-2 000 mg·L-1 and 50-800 mg·L-1, with detection limits (3S/N) of 106, 298 mg·kg-1, respectively. Test for recovery was made by the standard addition method, giving the results in the range of 92.4%-103%, with RSDs (n=6) of the determined values less than 3.0%. This method was used for the analysis of 4 actual samples, and ZPT was detected in only one indoor water-borne coating, with detection amount of 920 mg·kg-1.
中图分类号 O657.7 DOI 10.11973/lhjy-hx202312009
所属栏目 工作简报
基金项目 海关总署科研项目(2021HK223)
收稿日期 2023/3/10
修改稿日期
网络出版日期
作者单位点击查看
备注张琳,工程师,硕士,主要从事化工产品、涂料检测与标准化研究的工作
引用该论文: ZHANG Lin,YANG Juan,GUO Zhengyun,XU Jun,CHENG Yuxiao. Determination of Iodopropynyl Butylcarbamate and Zinc Pyrithione in Water-Borne Coating by High Performance Liquid Chromatography[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2023, 59(12): 1420~1424
张琳,杨娟,郭争云,徐骏,程欲晓. 高效液相色谱法测定水性涂料中碘丙炔醇丁基氨甲酸酯和吡啶硫酮锌的含量[J]. 理化检验-化学分册, 2023, 59(12): 1420~1424
共有人对该论文发表了看法,其中:
人认为该论文很差
人认为该论文较差
人认为该论文一般
人认为该论文较好
人认为该论文很好
参考文献
【1】彭红,谢小保,欧阳友生,等.涂料用防霉剂、抗菌剂和抗藻剂[J].中国涂料, 2007,22(12):48-52.
【2】季兴宏.生物杀伤剂在水性涂料中的应用及发展趋势[J].中国涂料, 2018,33(7):19-24.
【3】2014/312/EU:Commission decision of 28 May 2014 establishing the ecological criteria for the award of the EU Ecolabel for indoor and outdoor paints and varnishes (notified under document C(2014) 3429) text with EEA relevance[EB/OL].(2023-03-10)https://eur-lex.europa.eu/legal-content/EN/TXT/?uri=CELEX%3A32014D0312.
【4】中华人民共和国国家质量监督检验检疫总局,中国国家标准化管理委员会.绿色产品评价涂料:GB/T 35602-2017[S].北京:中国标准出版社, 2017.
【5】赵玥,李琼,张婉萍,等.高效液相色谱法对化妆品中低浓度碘丙炔醇丁基氨甲酸酯(IPBC)的检测[J].化学世界, 2011,52(2):87-91.
【6】杨艺欢.HPLC法测定皮革及皮革制品中防霉剂吡啶硫铜锌含量[J].山东化工, 2019,48(16):115-116.
【7】韩利平,王卿平,张景朋,等.IPBC高效液相色谱分析方法及处理材抗流失性能[J].北京林业大学学报, 2021,43(5):140-146.
【8】陶琳,薛秋红,叶曦雯,等.高效液相色谱法测定海洋涂料中吡啶硫酮锌[J].理化检验-化学分册, 2014,50(9):1109-1112.
【9】甘合智,韦东,张海殷.高效液相色谱法测定水性涂料中碘丙炔醇丁基氨甲酸酯[J].化学分析计量, 2022,31(6):18-22.
【10】蒋莹,蔡宇峰,赵霞,等.气相色谱法测定水性涂料中N,N-二(3-氨基丙基)十二烷基胺[J].化学试剂, 2021,43(10):1388-1392.
【11】杨艳伟,朱英,苏晓庆.高效液相色谱法测定去屑香波中水杨酸、吡啶硫酮锌吡啶酮乙醇胺、甘宝素和酮康唑5种去屑剂[J].卫生研究, 2005,34(5):626-628.
【2】季兴宏.生物杀伤剂在水性涂料中的应用及发展趋势[J].中国涂料, 2018,33(7):19-24.
【3】2014/312/EU:Commission decision of 28 May 2014 establishing the ecological criteria for the award of the EU Ecolabel for indoor and outdoor paints and varnishes (notified under document C(2014) 3429) text with EEA relevance[EB/OL].(2023-03-10)https://eur-lex.europa.eu/legal-content/EN/TXT/?uri=CELEX%3A32014D0312.
【4】中华人民共和国国家质量监督检验检疫总局,中国国家标准化管理委员会.绿色产品评价涂料:GB/T 35602-2017[S].北京:中国标准出版社, 2017.
【5】赵玥,李琼,张婉萍,等.高效液相色谱法对化妆品中低浓度碘丙炔醇丁基氨甲酸酯(IPBC)的检测[J].化学世界, 2011,52(2):87-91.
【6】杨艺欢.HPLC法测定皮革及皮革制品中防霉剂吡啶硫铜锌含量[J].山东化工, 2019,48(16):115-116.
【7】韩利平,王卿平,张景朋,等.IPBC高效液相色谱分析方法及处理材抗流失性能[J].北京林业大学学报, 2021,43(5):140-146.
【8】陶琳,薛秋红,叶曦雯,等.高效液相色谱法测定海洋涂料中吡啶硫酮锌[J].理化检验-化学分册, 2014,50(9):1109-1112.
【9】甘合智,韦东,张海殷.高效液相色谱法测定水性涂料中碘丙炔醇丁基氨甲酸酯[J].化学分析计量, 2022,31(6):18-22.
【10】蒋莹,蔡宇峰,赵霞,等.气相色谱法测定水性涂料中N,N-二(3-氨基丙基)十二烷基胺[J].化学试剂, 2021,43(10):1388-1392.
【11】杨艳伟,朱英,苏晓庆.高效液相色谱法测定去屑香波中水杨酸、吡啶硫酮锌吡啶酮乙醇胺、甘宝素和酮康唑5种去屑剂[J].卫生研究, 2005,34(5):626-628.
相关信息