建立了皮革及其皮革制品中痕量五氯苯酚的液相色谱同位素稀释质谱联用的检测方法.以酸化后的乙腈提取皮革及其皮革制品中残留的五氯苯酚,在 ZORBAX XDB-C18柱(50 mm伊2.1 mm,3.5滋m)上,采用(乙腈)颐(0.5豫乙酸水溶液)=75颐25(体积比)作为流动相进行分离,结合电喷雾电离 ESI离子化技术,在负离子 SIM 模式下测定,进行质谱定性分析,以13C-五氯苯酚为内标物进行定量,方法的定量限为0.005滋g/g,加标回收率为：91.0%~97.7%,重复次数=3时,测定精密度小于5%,以信噪比(S/N)为10计算,五氯苯酚的定量限(LOQ)为0.005滋g/g.方法准确、可靠,适用于皮革及其制品中痕量五氯苯酚残留的测定.%With acidified acetonitrifle as extraction, pentachlorophenol in leather and leather products was analyzed by liquid chromatography isotope dilution mass spectrometry in ZORBAX XDB-C18 column (50 mm í 2.1 mm, 3.5 μm). On chromatography separation step, acetonitrile and 0.5% aqueous solution of acetic acid (75:25, volume ratio) was used as the mobile phase. Combining of electrospray ionization ESI ionization technique, mass spectrometry qualitative analysis was determined on the anion SIM mode. By using 13C-pentachlorophenol phenol as internal standard, the quantitative limit is 0.005 μg/g, the adding standard recovery is (91.0 to 97.7)%. Keep the number of repetitions at 3, the relative standard deviation is less than 5% . If the signal -to -noise ratio (S/N) is 10, the limit of quantification (LOQ) of pentachlorophenol is 0.005 μg/g. The method is accurate, reliable, and suitable for the determination of trace residues of pentachlorophenol in leather and its products.
展开▼
