超高效液相色谱-质谱法测定水性涂料中的酚类防霉剂

Determination of Phenol Preservatives in Coating by Ultra High Performance Liquid Chromatography-Mass Spectrometry

建立了超高效液相色谱-质谱(UHPLC-MS)测定水性涂料中酚类防霉剂:邻苯基苯酚(OPP)、2,3,5,6-四氯苯酚(2,3,5,6-Te CP)、五氯苯酚(PCP)的方法。样品经甲醇提取后,采用ZORBAX SB-C18 Rapid Resolution HD(2.1 mm×50 mm,1.8-Micron)色谱柱分离,以甲醇/水为流动相进行梯度洗脱,电喷雾负离子模式(ESI-)电离,外标法定量。该方法具有良好的线性,分析线性范围为0.025~4.5 mg/L,相关系数为0.9994~0.9999,OPP、2,3,5,6-Te CP、PCP的方法检出限(LOD,S/N≥3)为0.275、0.08、0.15 mg/kg。在水性涂料基质中3个浓度水平的加标回收率为77.4%~108.9%,相对标准偏差为1.8%~9.7%(n=7)。方法具有样品处理方法简单、分析速度快、选择性好、灵敏度高等特点,适用于水性涂料产品中酚类防霉剂的检测分析。

A rapid method was developed for determination of o-Phenyl phenol, 2,3,5,6-tetrachlorophenol and pentachlorophenol in coating by ultra high performance liquid chromatography-mass spectrometry （UHPLC- MS）. Coating samples were extracted with methanol. Compounds were separated on ZORBAX SB-C18 Rapid Resolution HD（2.1 mm50 ×mm, 1.8-Micron）column, with CH3OH and water as mobile phase using gradient elution, and then determined with negative electrospray ionization mass spectrometry. The calibration curves of OPP, 2,3,5,6-TeCP and PCP showed good linear relationships in the range of 0.025-4.5 mg/L, with correlation coefficients of 0.9994-0.9999. The limits of detection （LOD, S/N≥3） were 0.275, 0.08, 0.15 mg/kg for OPP, 2,3,5,6-TeCP and PCP in coating. The average recoveries of compounds spiked at three concentration levels were in the range of 77.4 %-108.9 %, with the relative standard deviations （RSD） of 1.8 %-9.7 % （n=7）. The proposed method was simple, rapid, accurate, sensitive and suitable for determination of phenol preservatives in coating .