液相色谱-电喷雾质谱法测定污水和污泥中壬基酚聚氧乙烯醚的参数优化

在液相色谱-电喷雾质谱法测定壬基酚聚氧乙烯醚的过程中,对壬基酚聚氧乙烯醚加合离子的形成影响因素进行分析,优化了关键参数,建立了测定污水和污泥中壬基酚聚氧乙烯醚的高分辨高灵敏的液相色谱-电喷雾质谱方法.流动相A为0.1mmol·l~(-1)乙酸钠缓冲液,流动相B为甲醇,各聚合度壬基酚聚氧乙烯醚的加合离子响应值达到最大;锥孔电压没为60V能最大程度上避免NPnEO+2Na]~(2+)对测定的干扰.NP1EO,NP2EO和NPnEOs(n=3-15)的仪器检出限分别为10pg,1pg和0.1pg.该方法成功用于污水和污泥中壬基酚聚氧乙烯醚的测定.

OPTIMIZATION OF FACTORS DETECTING NONYLPHENOL ETHOXYLATES (NPnEOs) IN WASTEWATER AND SLUDGE BY LC-ESI-MS

The analysis of nonylphenol ethoxylate by liquid chromatography-electrospray ionization mass spectrometry (LC-ESI-MS) was investigated in terms of some parameters influencing the formation of different types of adducts. To compare the metal preference of NPnEOs during adduct formation, NaAc, NH_4Ac, and KAc were added to mobile phase, respectively, and the corresponding adducts were monitored. Results showed that the sodium adducts gave the most signals for both short-chain and long-chain oligomers at NaAc of 0.1 mmol ·l~(-1) used as the mobile phase buffer. At the cone voltage of 60V, NPnEO +2Na]~(2+) were eliminated at the most limit to avoid interference during quantification. For NP1EO, NP2EO, NPnEOs (n = 3-15), IDLs were 10pg, 1pg, 0.1pg, respectively. Investigation of NPnEOs in wastewater and sludge samples taken from a WWTPs in Beijing was successfully performed by this method.