水质 沉积物、悬浮颗粒物和生物群中多溴联苯醚(PBDE)的测定 气相色谱联用串联质谱(GC-MS/MS)或高分辨率质谱(GC-HRMS)方法

[中文适用范围]： 本文件规定了一种使用气相色谱串联质谱法（GC-MS/MS）或高分辨质谱法（GC-HRMS），在电子轰击（EI）、负离子化学电离（NCI）或大气压化学电离（APCI）模式下，测定沉积物、悬浮颗粒物和生物体中选定多溴二苯醚（PBDE）的方法。该方法适用于沉积物和悬浮颗粒物样品，BDE-28至BDE-183的定量限为0.2 µg/kg干重（dm），BDE-209的定量限为2 µg/kg干重（dm）。如果结合使用第10章表3所述的方法1和方法2等特定净化方法，并配合GC-MS/MS或GC-HRMS测量方法（针对BDE-209采用电子轰击电离或负离子化学电离），则可获得更低的定量限。根据仪器的分析能力，BDE-28至BDE-154的定量限可低至0.003 µg/kg dm，BDE-183和BDE-209的定量限可低至0.02 µg/kg dm和1 µg/kg dm。该方法适用于生物体样品，如果结合使用表4所述的特定净化方法，并配合GC-MS/MS或GC-HRMS测量方法（针对BDE-209采用电子轰击电离），则BDE-28至BDE-154的定量限可低至0.0002 µg/kg鲜重（fm），BDE-183的定量限可低至0.03 µg/kg鲜重（fm）。性能数据列于附件E。 [外文原描述]： This document specifies a method for the determination of selected polybrominated diphenylethers (PBDE) (see Figure 1 and Table 1 ) in sediment, suspended particulate matter and biota using gas chromatography coupled with tandem mass spectrometry (GC-MS/MS) or with high resolution mass spectrometry (GC-HRMS) in the electron impact (EI), negative ion chemical ionization (NCI) or atmospheric pressure ionization (APCI) mode. The method is applicable to sediment and suspended particulate matter samples with limits of quantification of 0,2 µg/kg dry mass (dm) for brominated diphenylether (BDE) BDE-28 to BDE-183, of 2 µg/kg dry mass (dm) for BDE‑209. The method is applicable as well with lower limits of quantification (LOQ), if specific clean-up methods, described in Clause 10 , Table 3 , method 1 and method 2 in combination with measurement methods GC-MS/MS or GC-HRMS after electron impact ionization (El) or negative ion chemical ionization (NCI) for BDE-209 are used. Depending on the analytical capability of the instrument, limits of quantification down to 0,003 µg/kg dm for BDE-28 to BDE-154 and 0,02 µg/kg dm for BDE-183 and 1 µg/kg dm for BDE-209 and lower are possible. The method is applicable to biota samples with limits of quantification down to 0,000 2 µg/kg fresh mass (fm) (BDE-28 to BDE-154) and 0,03 μg/kg fresh mass (fm) (BDE-183), if specific clean-up methods, described in Table 4 in combination with measurement methods GC-MS/MS or GC-HRMS after electron impact ionization (El) are used. Performance data are listed in Annex E .