Jeannot Roger, Sabik Hassan, Sauvard Emmanuel, Dagnac Thierry, Dohrendorf Katja
Service Analyse et Caractérisation Minérale, BRGM, BP 6009, 45060 Orleans Cedex 02, France.
J Chromatogr A. 2002 Oct 18;974(1-2):143-59. doi: 10.1016/s0021-9673(02)01240-2.
This paper describes certain applications for endocrine-disrupting compounds determination. LC-MS was applied using an electrospray ionization (ESI) technique in positive mode for alcohol polyethoxylates and nonylphenol and octylphenol polyethoxylates (NPEOn and OPEOn), and in negative mode for 4-nonylphenol (4-NP) and 4-octylphenol (4-OP) to determine targeted compounds in wastewater and sludge. GC-MS and GC-MS-MS were used to determine 4-NP, 4-tert.-octylphenol (4-t-OP), bisphenol A, estradiol-17beta, estriol estrone, testosterone, 17alpha-ethynylestradioL cholesterol, coprostan-3-ol, coprostan and coprostan-3-one in both surface water and wastewater after derivatization with N,O-bis(trimethyl-silyl)trifluoroacetamide (BSTFA). Extraction from the water samples was by an SPE technique, using either a copolymeric (Oasis HLB) or C18 silica sorbents, depending on the target contaminants. Extraction from the sludge samples was by a Soxtec system using methanol. Percentage recoveries for most of the selected compounds, using either a copolymeric (Oasis HLB) or C18 silica sorbents, were satisfactory (>60%). Quantification limits for the target compounds were at ppb levels in both water and sludge samples when using LC-ESI-MS in both positive and negative modes. They reached ppt levels in water when using GC-MS (in large volume injection mode) and GC-MS-MS. The results revealed 4-NP, NPEOn and AEOs in sludge samples at a concentration range of 1.3-8.5 microg/g, and NPEOn, OPEOn and other compounds, such as coprostan and bisphenol A, in surface water and/or wastewater samples at concentrations ranging from the ppt to ppb levels.
本文描述了内分泌干扰化合物测定的某些应用。采用液相色谱 - 质谱联用（LC-MS），使用电喷雾电离（ESI）技术，在正模式下测定醇聚乙氧基化物、壬基酚和辛基酚聚乙氧基化物（NPEOn和OPEOn），在负模式下测定4-壬基酚（4-NP）和4-辛基酚（4-OP），以测定废水和污泥中的目标化合物。气相色谱 - 质谱联用（GC-MS）和气相色谱 - 串联质谱联用（GC-MS-MS）用于在使用N，O-双（三甲基硅基）三氟乙酰胺（BSTFA）衍生化后，测定地表水和废水中的4-NP、4-叔辛基酚（4-t-OP）、双酚A、雌二醇-17β、雌三醇、雌酮、睾酮、17α-乙炔基雌二醇、胆固醇、粪甾烷-3-醇、粪甾烷和粪甾烷-3-酮。水样的萃取采用固相萃取（SPE）技术，根据目标污染物的不同，使用共聚体（Oasis HLB）或C18硅胶吸附剂。污泥样品的萃取采用索氏提取系统，使用甲醇。使用共聚体（Oasis HLB）或C18硅胶吸附剂时，大多数选定化合物的回收率令人满意（>60%）。使用正负极模式的LC-ESI-MS时，水和污泥样品中目标化合物的定量限均为ppb级别。使用GC-MS（大体积进样模式）和GC-MS-MS时，水中的定量限达到ppt级别。结果显示，污泥样品中4-NP、NPEOn和脂肪醇聚氧乙烯醚（AEOs）的浓度范围为1.3 - 8.5微克/克，地表水和/或废水样品中NPEOn、OPEOn以及其他化合物，如粪甾烷和双酚A的浓度范围为ppt至ppb级别。
