超声萃取-气相色谱-质谱联用法测定船舶用材料中6种多氯化萘

多氯化萘(PCNs)是船舶有害物质清单中的必测项目，目前并没有统一的检测标准，因此建立一种适用于船舶用材料中多氯化萘的方法十分有必要。选取船舶用材料，以丙酮-正己烷混合溶液为萃取溶剂，超声萃取1 h,过滤后，采用Agilent&HP-5MS(30 m×0.25 mm×0.25μm)毛细管柱进行分离，四极杆质谱检测器分析检测，实现了气相色谱-质谱联用法(GC-MS)对样品中6种多氯化萘的测定。方法的线性范围为10～100μg/L,校准曲线的相关系数均大于0.998,检出限在14.0～40.6μg/kg之间，定量限在46.8～135.3μg/kg之间。分别在PCNs含量低于检出限的船舶用材料中加入200、500、900μg/kg共3个含量水平的PCNs,结果表明，6种PCNs的加标回收率为99%～109%,相对标准偏差(RSD,n=6)为0.29%～4.2%。按照实验方法和已有文献中的方法分别对3种船舶用材料(电容器、电缆、润滑油)中6种PCNs进行分析，加标含量为500μg/kg,方法的回收率为98%～105%,相对标准偏差(n=6)为1.7%～3.8%。

Determination of 6 polychlorinated naphthalene in marine material by gas chromatography-mass spectrometry with ultrasonic extraction

Polychlorinated naphthalenes(PCNs) are items that must be detected in the list of hazardous substances in ship. At present, there is no united test standard, so it is necessary to establish a method for the determination of PCNs in marine materials. The marine material was treated by ultrasonic extraction for 1 h with acetone-normal hexane mixed solvent. After filtration, Agilent and HP-5MS (30 m×0.25 mm×0.25 μm) capillary column was used for separation. Quadrupole mass spectrometry detector was employed for quantitative analysis. The determination of six PCNs in sample was realized by gas chromatography-mass spectrometry(GC-MS). The linear range of method was 10-100 μg/L. The correlation coefficients of calibration curve were all higher than 0.998. The limits of detection were 14.0-40.6 μg/kg, and the limits of quantification were 46.8-135.3 μg/kg. Three content levels of PCNs (200, 500 and 900 μg/kg) were added into marine materials with content lower than the limit of detection. The results showed that the recoveries of six PCNs were between 99% and 109%. The relative standard deviations (RSD, n=6) were between 0.29% and 4.2%. Six PCNs in three marine materials (capacitor, cable and lubricating oil) were analyzed according to the experimental method and existing method in the literature. The standard addition content was 500 μg/kg. The recoveries of method were between 98% and 105%. The RSD(n=6) were between 1.7% and 3.8%.