Occurrence and fate of steroid estrogens in the largest wastewater treatment plant in Beijing, China

Concern over steroid estrogens has increased rapidly in recent years due to their adverse health effects. Effluent discharge from wastewater treatment plants (WWTPs) is the main pollutant source for environmental water. To understand the pollutant level and fate of steroid estrogens in WWTPs, the occurrence of estrone (E1), 17-β-estradiol (E2), estriol (E3), and 17-β-ethinylestradiol (EE2) was investigated in the Gaobeidian WWTP in Beijing, China. Water samples from influent as well as effluent from second sedimentation tanks and advanced treatment processes were taken monthly during 2006 to 2007. In influent, steroid estrogen concentrations varied from 11.6 to 1.1?×?10(2)?ng/l, 3.7 to 1.4?×?10(2)?ng/l, no detection (nd) to 7.6×10(2)?ng/l and nd to 3.3?×?10(2)?ng/l for E1, E2, E3, and EE2, respectively. Compared with documented values, the higher steroid estrogen concentrations in the WWTP influent may be due to higher population density, higher birthrate, less dilution, and different sampling time. Results revealed that a municipal WWTP with an activated sludge system incorporating anaerobic, anoxic, and aerobic processes could eliminate natural and synthetic estrogens effectively. The mean elimination efficiencies were 83.2%, 96.4%, 98.8%, and 93.0% for E1, E2, E3, and EE2, respectively. The major removal mechanism for natural estrogens and synthetic estrogen EE2 were biodegradation and sorption on the basis of mass balance in water, suspension particles, and sludge. In the WWTP effluent, however, the highest concentrations of E1, E2, E3, and EE2 attained were 74.2, 3.9, 5.1, and 4.6?ng/l, respectively. This is concerning as residual steroid estrogens in WWTP effluent could lead to pollution of the receiving water. Advanced flocculation treatment was applied in the WWTP and transformed the residual estrogen conjugates to free species, which were reduced further by filtration with removal shifting from 32% to 57% for natural estrogen, although no EE2 was removed.     

Dynamics of steroid estrogen daily concentrations in hospital effluent and connected waste water treatment plant

Hospital effluent and connected waste water treatment plant (WWTP) influent and effluent were sampled daily to determine the levels and inter-day variations of three naturally occurring steroid estrogens: estrone, 17β-estradiol, estriol, and synthetic 17α-ethinylestradiol. After solid phase extraction, interferences were removed with a silica gel clean-up step and the samples analysed using gas chromatography with mass selective detection (GC-MSD). The determined inter-day concentrations in hospital effluent were between 8.6 to 31.3 ng L(-1) for estrone, 相似文献   

An alternative method for the determination of estrogens in surface water and wastewater treatment plant effluent using pre-column trimethylsilyl derivatization and gas chromatography/mass spectrometry

A procedure using pre-column trimethylsilyl derivatization and gas chromatography/ mass spectrometry (GC/MS) was developed and applied in determining trace estrogens in complex matrix. Main conditions were optimized, including pH value, salinity of water sample, elution reagents, clean procedure, derivative solvent and temperature. The optimized method was used to determine steroid estrogens in surface water and effluents of wastewater treatment plant (WWTP). Low detection limits of 0.01, 0.03, 0.03, 0.07, 0.09 and 0.13 ng/l for DES, E1, E2, EE2, E3 and E(V), respectively were obtained under optimism condition. No apparent interferences appeared in chromatography in comparison with ultrapure water blank. Mean recovery ranged from 72.6% to 111.0% with relative standard deviation of 1.1-4.6% for spiked surface water, and from 66.6% to 121.1% with relative standard deviation of 1.5-4.7% for spiked effluent of WWTP. The results suggested that the optimized method provides a robust solution for the determination of trace steroid estrogens in complex matrix.     

Occurrences of six steroid estrogens from different effluents in Beijing, China

Concentration levels of six natural and anthropogenic origin steroid estrogens, namely, diethylstilbestrol (DES), estrone (E1), estradiol (E2), estriol (E3), ethinylestradiol (EE2), and estradiol-17-valerate (Ev), from different effluents in Beijing were assessed. Sampling sites include two wastewater treatment plants (WWTPs), a chemical plant, a hospital, a pharmaceutical factory, a hennery, and a fish pool. In general, concentrations of estrogens in the effluents varied from no detection (nd) to 11.1 ng/l, 0.7 to 1.2 × 10³ ng/l, nd to 67.4 ng/l, nd to 4.1 × 10³ ng/l, nd to 1.2 × 10³ ng/l, and nd to 11.2 ng/l for DES, E1, E2, EE2, E3, and Ev, respectively. The concentration levels of steroid estrogens from different effluents decreased in the order of pharmaceutical factory and WWTP inlets > hospital > hennery > chemical factory > fish pool. This study indicated that natural estrogens E1, E2, and E3 and synthetic estrogen EE2 are the dominant steroid estrogens found in the different Beijing effluents. For source identification, an indicator (hE = E3/(E1 + E2 + E3)) was used to trace human estrogen excretion. Accordingly, hE in effluents from the hospital and WWTP inlets exceeded 0.4, while much smaller values were obtained for the other effluents. Human excretions were the major contributor of natural estrogens in municipal wastewater. Estimation results demonstrated that direct discharge was the major contributor of steroid estrogen pollution in receiving waters.     

徐州市污水厂内分泌干扰物的去除及生态风险评价

对徐州市3家不同处理工艺污水厂进出水中的17α-乙炔基雌二醇(EE2)、雌三醇(E3)、雌二醇(E2)、雌酮(E1)、双酚A(BPA)等5种雌激素物质进行了分析,采用固相萃取技术对这些物质进行富集分离,使用LC-MS对目标物进行检测。结果表明,3座污水厂的雌激素(除BPA)平均进出水浓度较高,污水厂对EE2和BPA的去除效果较好,分别为84.89%和98.38%;但对E3、E2、E1去除效果不够理想。经对内分泌干扰物的雌激素活性及生态风险进行评价,建议徐州地区应优先控制EE2、E1和E3。     

Occurrence and fate of androgens, estrogens, glucocorticoids and progestagens in two different types of municipal wastewater treatment plants

The occurrence and fate of fourteen androgens, four estrogens, five glucocorticoids and five progestagens were investigated in two different types of wastewater treatment plants (Plant A: activated sludge with chlorination, and Plant B: oxidation ditch with UV) of Guangdong province, China. 14, 14, and 10 of 28 target compounds were detected in the influent, effluent and dewatered sludge samples with the concentrations ranging from below 1.2 ± 0.0 ng L(-1) (stanozolol) to 1368 ± 283 ng L(-1) (epi-androsterone), below 1.0 ± 0.0 ng L(-1) (progesterone) to 23.1 ± 1.0 ng L(-1) (5α-dihydrotestosterone), 1.0 ± 0.1 ng g(-1) (estrone) to 460 ± 4.4 ng g(-1) (5α-dihydrotestosterone), respectively. The concentrations of total androgens (1554-1778 ng L(-1) in influent, 13.3-47.8 ng L(-1) in effluent, 377-923 ng g(-1) in dewatered sludge) were much higher than those of total estrogens (41.5-60.2 ng L(-1) in influent, 5.6-13.5 ng L(-1) in effluent, 13.9-57.8 ng g(-1) in dewatered sludge), glucocorticoids (171-192 ng L(-1) in influent, 2.2-6.3 ng L(-1) in effluent, N.D.-4.4 ng g(-1) in dewatered sludge), and progestagens (39.6-40.5 ng L(-1) in influent, 6.9-12.1 ng L(-1) in effluent, N.D. in dewatered sludge) in these two WWTPs. According to mass balance analysis, the removal rates of most target steroids in Plant A had exceeded 90%, while those in Plant B for nearly half of detected target steroids were lower than 80%. It is obvious that the treatment capacity of the activated sludge system (Plant A) is superior to the oxidation ditch (Plant B) in the degradation of steroids in sewage treatment systems. Androgens, estrogens and progestagens were mainly removed by sorption and degradation, while the reduction of glucocorticoids was primarily due to degradation.     

液相色谱-串联质谱法同时测定污水中10种精神活性物质

建立了采用液相色谱-串联质谱法(LC-MS/MS)同时测定污水中10种精神活性物质的分析方法。污水样品经甲酸与甲酸铵调节pH后,加入氘代内标混匀,离心并过滤膜后可直接上样分析。研究表明,在1~250 ng/L的线性范围内,10种精神活性物质的线性相关系数均大于0.992,定量限均低于0.5 ng/L。在3个加标水平下,10种精神活性物质的加标回收率为87.2%~114%,相对标准偏差为0.53%~3.60%(n=3)。将该方法应用于某区域10份生活污水样品的检测,在3份水样中检出吗啡、甲基苯丙胺、氯胺酮等精神活性物质,对应的质量浓度范围分别为3.41~9.55、0.90~1.63、1.06~1.78 ng/L。与经固相萃取前处理后的分析方法相比,该方法可在10 min内完成分离和检测的全过程,具有简单、快速、节约的优点,可用于污水样品中10种痕量水平精神活性物质的定量分析。     

Behaviour of selected endocrine-disrupting chemicals in three sewage treatment plants of Beijing, China

Occurrence and fate of eight kinds of selected endocrine-disrupting compounds (EDCs) in three sewage treatment plants (STPs) of Beijing, China was investigated. These EDCs, composed of 4-octylphenol (4-OP), 4-n-nonylphenol (4-n-NP), bisphenol A (BPA), estrone (E1), 17α-estradiol (17α-E2), 17β-estradiol (E2), estriol (E3) and 17α-ethinylestradiol (EE2), in every step of STPs, were simultaneously analysed by gas chromatography/mass spectrometry after derivatisation. All the EDCs were detected in the influents of three STPs, and BPA was the most abundant compound. The concentrations of EDCs ranged from 36.6 ng/l of 17α-E2 (STP C) to 1342.3 ng/l of BPA (STP B) in the influent sewages and from below limits of detection of E2 and E3 (STP C) to 142.5 ng/l of E1 (STP B) in the effluent sewages. The STPs could not remove alkylphenols effectively from the aqueous phase with less than 40% reduction. BPA decreased over 90%, and steroid estrogens achieved considerable reductions from 64.8% of E2 to 94.9% of E3. Generally, biological treatment was more effective in removing alkylphenols, BPA and natural estrogens from the aqueous phase than primary treatment. However, the synthetic estrogen, EE2, was mostly removed by the primary treatment with about 63.5% reduction. It is the first time that the concentration of 17α-E2 in the sewage of China was reported in this paper. The compound might have a bearing with the waste effluents of dairy farms around urban area of Beijing.     

Effect of process conditions on the analysis of free and conjugated estrogen hormones by solid-phase extraction–gas chromatography/mass spectrometry (SPE–GC/MS)

Simultaneous analysis of 11 free estrogen hormones and five conjugated estrogens in water and municipal wastewater was studied. The analytical method was developed and tested for different types of solid-phase extraction adsorbents, eluents, sample containers and storage conditions, derivatization, and matrix effects. Varian Bond Elut C-18 solid-phase extraction adsorbent cartridge was selected based on its high recoveries for both free and conjugated estrogens. Sample storage conditions, as well as selection and pretreatment of sample container materials, can affect the trace level analysis of estrogens. Silanization of glassware is observed to provide low relative standard deviation (RSD) in the analysis and less percentage loss due to contacting with sample container materials. Light exposure during the test can significantly impact the results. The derivatized samples stored at −20°C for at least 6 days showed less than 10.5% average RSD in the analysis. The recovery efficiency in clean water varies from 72% to 101% for free estrogens and 78% to 82% for conjugated estrogens. The method detection limits (MDL) for most of the compounds range from 30 to 870 ng/L using a sample volume of 200 mL. With a sample volume of 3 L, the most sensitive compound produces a MDL of 0.03 ng/L. Dilute methanol is used to wash the loaded cartridge as a cleanup step in order to remove interfering species during analysis of wastewater samples. Using the optimized analytical methods, the concentration level of free estrogens in the influent and effluent municipal wastewaters is tested.     

Occurrence and removal of endocrine-disrupting chemicals in wastewater treatment plants in the Three Gorges Reservoir area, Chongqing, China

Concentrations of six endocrine-disrupting compounds (EDCs), bisphenol A (BPA), estrone (E(1)), 17β-estradiol (E(2)), estriol (E(3)), 17α-ethynylestradiol (EE(2)) and diethylstilbestrol (DES), were assessed in influents, effluents and excess sludge in ten municipal wastewater treatment plants (WWTPs) in the Three Gorges Reservoir (TGR) area, Chongqing, China. Three types of activated sludge treatment processes, oxidation ditch (OD), reversed anaerobic-anoxic-oxic (rA(2)/O) technology and sequential batch reactor (SBR), were used in the surveyed WWTPs. These WWTPs were all combined landfill leachate-sewage treatment plants. All analytes were extracted by solid-phase extraction (SPE) in the dissolved phase and by accelerated solvent-based extraction (ASE) in sludge. Gas chromatography-mass spectrometry (GC-MS) was employed for the analysis of EDCs. Among these EDCs, BPA was the most frequently detected and abundant compound (100.0-10566.7 ng L(-1), 15.5-1210.7 ng L(-1) and 85.0-2470.4 ng g(-1) with respect to the influents, effluents and excess sludge samples). The greatest levels of steroidal estrogens in municipal influents were observed in E(3) which were all >100 ng L(-1), followed by E(1) (42.2-110.7 ng L(-1)) and E(2) (7.4-32.7 ng L(-1)), and in the effluents and sludge were E(1) > E(3) > E(2) which were all <31 ng L(-1) and 105 ng g(-1), respectively. Regarding synthetic estrogens, EE(2) was frequently detected in the influents, occurring below 50 ng L(-1), while DES was not detected at all. A high correlation coefficient was observed between the leachate-sludge ratio and concentrations of influent EDCs, and it was statistically significant (i.e., R > 0.65, P < 0.05), but removal efficiency of the EDCs did not show significant differences with OD, rA(2)/O and SBR processes. Furthermore, modification of treatment technology as well as operational parameters, such as hydraulic retention time (HRT), sludge retention time (SRT) and disinfection process (DP), were recommended to further eliminate the residual EDCs.     

Determination of micropollutants in combined sewer overflows and their removal in a wastewater treatment plant (Seoul,South Korea)

The present study investigated the occurrence of 29 selected micropollutants such as endocrine disrupting compounds (EDCs) and pharmaceuticals and personal care products (PPCPs) in surface waters and wastewaters in Seoul (South Korea) during both dry and wet weather conditions. The study area was selected based on the lack of available information regarding the suspected contamination of rivers/creeks by EDCs and PPCPs in the Seoul region and the presence of a wastewater treatment plant (WWTP), which serves approximately 4.1 million inhabitants and has a design capacity of 1,297?×?10³ m³/day. Many target compounds (83 %) were detected in samples collected from wastewater treatment influent/effluent, creek water, and combined sewer overflow (CSO). The total EDC/PPCP concentrations were as follows: WWTP influent (69,903 ng/L)?>?WWTP effluent (50,175 ng/L) >3 creek samples (16,035–44,446 ng/L) during dry weather, and WWTP influent (53,795 ng/L)?>?WWTP bypass (38,653 ng/L) >5 creek samples (15,260–29,113 ng/L) >2 CSO samples (11,109–11,498 ng/L) during wet weather. EDCs and PPCPs were found to be present at high daily loads (65.1 and 69.8 kg/day during dry and wet weather, respectively) in the WWTP effluent. Compound removal by the WWTP varied significantly by compound: caffeine, diclofenac, ibuprofen, naproxen, and propylparaben (>90 %), and acesulfame, DEET, iohexol, iopromide, and iopamidol (<5 %). These findings and literature information support the hypothesis that the efficiency of removal of EDCs and PPCPs is strongly dependent on both removal mechanism (e.g., biodegradation, adsorption to sludge, and oxidation by chlorine) and compound physicochemical properties (e.g., pK _a and hydrophobicity).     

Occurrence of estrogenic chemicals in South Korean surface waters and municipal wastewaters

Broad scale monitoring of estrogenic compounds was performed at 19 sampling points throughout the Yeongsan and Seomjin river basins and 5 wastewater treatment plants (WWTPs) adjacent to the Gwangju area, Korea, from December 2005 to August 2007. The concentrations of estrogenic compounds, including estrone (E1), 17β-estradiol (E2), 17α-ethynylestradiol (EE2), bisphenol-A, nonylphenol (NP) and 4-octylphenol (OP), in the samples was measured with gas chromatography/mass spectrometry (GC-MS). In addition, the estrogenic activities throughout the river were investigated using the E-screen assay. Of the six estrogenic chemicals, NP (114.6-336.1 ng L(-1)) and EE2 (0.23-1.90 ng L(-1)) were detected at the highest and lowest levels, respectively in both the river waters and the WWTP effluents. Bisphenol-A showed the largest concentration range, from 7.5 to 335 ng L(-1). The concentrations of E1, E2 and octylphenol ranges were 3.6-69.1, 1.2-10.7, and 2.2-16.9 ng L(-1), respectively. According to the calculated estradiol equivalent concentration (EEQ); however, no estrogenic contribution was observed due to the phenolic compounds in the river waters and effluents. E1 and E2 dominated in both the river water and effluent samples, with contributions to the calculated EEQ of over 79 and 77%, respectively. Conversely, EE2 was rarely detected in the river waters (21%) and effluents (0%). The largest contribution of EE2 to the calculated EEQ was 21% in the river water at S-7. The levels of E1, E2, and EE2 were remarkably decreased in the effluents, indicating that the 5 WWTPs did not contribute to the estrogenic effect of the receiving streams. Overall, the WWTPs did not contributed to the estrogenic activity of the receiving waters, but the livestock industry or wildlife may play an important role in the estrogenic contribution to river water.     

In situ polar organic chemical integrative sampling (POCIS) of steroidal estrogens in sewage treatment works discharge and river water

A passive sampler (the polar organic chemical integrative sampler; POCIS) was assessed for its ability to sample natural estrogens (17β-estradiol, E2; estrone, E1 and estriol, E3) and the synthetic estrogen (17α-ethynylestradiol, EE2) in the outlet of a sewage treatment works over several weeks. The performance of the POCIS was investigated and optimised in the laboratory before field deployment with high recoveries (66-99%) were achieved for all estrogens. Moreover, it was shown that POCIS does not exhibit any preferential selectivity towards any of the target compounds. The sampling rates of E1, E2 and E3 were 0.018 ± 0.009, 0.025 ± 0.014 and 0.033 ± 0.019 L d(-1), respectively. Following field deployments of 28 days in the discharge of a sewage works, POCIS was shown to enhance the sensitivity of estrogen detection, especially for E3, and provide time-weighted average (TWA) concentrations of E1, E2 and E3, ranging from undetectable to 12 ng L(-1) upstream of the outflow of a sewage treatment works, 13 to 91 ng L(-1) at the outflow and 8 to 39 ng L(-1) downstream of the outflow. This revealed that E1, E2 and E3 are not completely removed during sewage treatment, with concentrations most likely being maintained by contributions from conjugated estrogen analogues. Grab water samples showed considerable variation in the concentrations of estrogens over a longer period (6 months). The results confirm that POCIS is an effective and non-discriminatory method for the detection of low concentrations of estrogens in the aquatic environment.     

Occurrence and distribution of benzothiazole in the Schwarzbach watershed (Germany)

This study quantifies the regional distribution of the micropollutant benzothiazole (BT) in river water by sampling 15 river sites in the Schwarzbach watershed (about 400 km(2)) from November 2008 to February 2010. Additionally, wastewater samples from three municipal wastewater treatment plants (WWTPs) in Germany were analyzed. BT was detected in all wastewater influent and effluent samples as well as in all river water samples collected downstream of wastewater discharge. This corroborates the ubiquitous occurrence of BT in the aqueous environment. Concentrations were between 58 and 856 ng L(-1) in the river water. The observed mean concentration at the outlet of the investigated catchment was 109 ng L(-1). With only a few exceptions, temporal and spatial variations of BT concentrations in river water were low. Rather similar BT concentrations over a wide range of river discharge indicate that dilution along the mainstream is negligible and, thus, supports the hypothesis that paved surface runoff during rain events is an important BT source not only for wastewater influent but also for river water. This was supported by detecting the highest BT concentrations at sampling locations close to the dense highway network around the city of Frankfurt. Since BT was also detected in river water collected from locations that were clearly unaffected by wastewater effluent discharge, surface runoff must be considered as a diffuse source of BT in river water.     

Migration of natural estrogens around a concentrated dairy-feeding operation

Concentrated animal feeding operations have been recognized as one of the most important contributors of natural estrogens which show significant endocrine-disrupting properties in aquatic environments. In this study, the concentrations of 17α-estradiol (17α-E2), 17β-estradiol (17β-E2), estrone (E1), and estriol (E3) in several matrices, including soils (surface and deep), sediments (surface and deep), and groundwaters, around a typical dairy farm were surveyed using gas chromatography/mass spectrometry. Of the two farmlands, surface and subsurface sediments in waste lagoon and along effluent drainage drench, the concentrations of 17α-E2, 17β-E2, and E1 ranged from below detection limit to the highest level of 6.60 μg/kg, except that E3 was not detectable. Three estrogens of 17α-E2, 17β-E2, and E1 with the concentrations of 3.18-31.61 ng/L were observed in two groundwater samples. The results clearly demonstrated the vertical migration and horizontal transport of estrogens in the investigated area. Within 750-m distance, it was observed the attenuation of 17α-E2, 17β-E2, and E1 along the effluent route and the horizontal migration of estrogens was less than 1,350 m in this survey.     

Occurrence and removal efficiencies of eight EDCs and estrogenicity in a STP

The occurrence and removal of eight endocrine disrupting compounds (EDCs), including estrone (E(1)), 17β-estradiol (E(2)), estriol (E(3)), 17α-ethinylestradiol (EE(2)), diethylstilbestrol (DES), bisphenol A (BPA), nonylphenol (NP) and octylphenol (OP), and their estrogenicities were investigated in a sewage treatment plant in Harbin city, China. The EDCs were extracted from wastewater samples by solid phase extraction (SPE) method and analyzed with gas chromatography coupled with mass spectrometry (GC-MS). The average concentrations in the influents and effluents ranged from 6.3 (EE(2)) to 1725.8 ng L(-1) (NP) and from 相似文献   

SBSE-GC/MS法测定饮用水源水中7种多氯联苯单体

采用搅拌棒吸收萃取(SBSE)-溶剂解吸-气相色谱/质谱联用法测定饮用水源水中7种多氯联苯单体,优化了萃取和解吸条件。方法在5 ng/L~100 ng/L范围内线性良好(r≥0.979),7种多氯联苯单体的检出限为0.8 ng/L~3.4 ng/L(100 mL水样SBSE萃取2 h),加标10 ng/L时实际水样回收率为93.0%~116%。     

Assessment of current status of zinc in wastewater treatment plants to set effluent standards for protecting aquatic organisms in Japan

New environmental standards for protecting aquatic organisms for zinc (e.g., 0.03 mg/L) in surface waters were set in Japan in 2003. Although wastewater effluent might be one of the major pathways of zinc to public water bodies in Japan, current status of concentration of zinc in wastewater effluent was not clear due to higher detection limits (e.g., 0.5 mg/L) than the level required by the new regulations. This study aims at assessing current status of zinc in wastewater effluent in Japan to revise wastewater effluent standards for protecting aquatic organisms. Survey of zinc in wastewater treatment plants (WWTPs) was carried out in Japan in 2005, setting the detection limits at least 0.01 mg/L. The results of the survey suggested the difficulty to remove zinc (especially dissolved zinc) with conventional activated sludge treatment if concentration of zinc in influent was relatively low. And it was suggested that high concentration of dissolved zinc might be derived from some industries discharging high concentration of zinc. The concentration of zinc in wastewater influent without industrial discharges was about 0.1 mg/L which might be lower than that in wastewater from industries discharging high concentration of zinc. Finally, effluent standards for point sources including WWTPs to public water bodies were set at 2 mg/L in 2006. Based on the results of the survey that it was difficult to remove dissolved zinc discharged from industries at WWTPs, the effluent standards from industries to sewerage were set at the same value of the effluent standards from WWTPs to public water bodies.     

水中微囊藻毒素的超高效液相色谱-串联质谱法研究

建立测定水体中微囊藻毒素(MCYST)的超高效液相色谱-串联质谱分析方法.水样通过固相萃取富集净化,采用超高效液相色谱-串联质谱测定,6min内完成3种MCYST的分离及检测.MCYST-LR、MCYST-RR、MCYST-YR检出限分别为3.5、2.5、5.0ng/L,回收率为85.6％～107.9％,为水质微囊藻毒素监测提供了一种快速、准确、灵敏的分析方法.     

水体中磺胺、四环素、喹诺酮类抗生素检测方法

建立了固相萃取-高效液相色谱-串联质谱法(SPE-HPLC-MS/MS)同时检测水体中3类15种抗生素的分析方法。水样用Oasis HLB固相萃取小柱净化富集。通过对比水样在不同pH条件下的回收率,优化了环境水样中抗生素固相萃取过程中的前处理条件。采用甲醇和0.1%甲酸溶液作为流动相,经过梯度洗脱进行分离,在HPLC-MS/MS多反应监测模式下进行定性定量分析。结果表明,环境水体中15种抗生素的检出限和定量下限分别为0.12~1.6 ng/L和0.2~3.0 ng/L,自来水加标回收率为34.9%~102.5%(pH=4)。用该方法对海河流域13个地表水水样进行了初步检测,结果表明,部分抗生素普遍存在于地表水体中。其中,磺胺甲基异NFDA1唑检出频率最高,在13个地表水样品中均有检出。