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目的 建立一种全自动固相萃取-液相色谱串联质谱法同时测定饮用水中21种有机磷酸酯(organophosphate esters, OPEs)及其代谢产物的方法。方法 饮用水加入内标后，采用HLB固相萃取柱，全自动固相萃取净化，甲醇洗脱，采用ACQUITY UPLC BEH(100 mm×2.1 mm, 1.7μm)色谱柱，液相色谱串联质谱法测定，内标法定量。结果 优化后的方法可以同时检测饮用水中21种有机磷酸酯及其代谢产物，检出限为0.01～0.24 ng/L,定量限为0.03～0.77 ng/L,加标0.8～20 ng/L,回收率范围为57.6%～121.2%,相对标准偏差为1.2%～11.1%(n=6)。对17件市政末梢水及30件商超采集的包装饮用水进行测定，ΣOPEs范围为16.8～177 ng/L,Σdi-OPEs范围为0.328～16.3 ng/L,说明水体存在有机磷酸酯及其代谢产物的暴露风险。结论 本法前处理自动化程度高、简单，灵敏度高，适用于大批量饮用水中有机磷酸酯及其代谢产物的同时高通量测定。
Abstract：OBJECTIVE To establish a method for simultaneous determination of 21 organophosphate esters(OPEs) and their metabolites in drinking water by automatic solid phase extraction-liquid chromatography-tandem mass spectrometry.METHODSThe drinking water was purified by automatic solid phase extraction with HLB column, eluted by methanol, determined by liquid chromatography tandem mass spectrometry with ACQUITY UPLC BEH(100 mm×2.1 mm, 1.7 μm) column, and quantified by internal standard method.RESULTS The optimized method could simultaneously detect 21 organophosphate esters and their metabolites in drinking water. The detection limit was 0.01-0.24 ng/L, the quantitation limit was 0.03-0.77 ng/L. The recovery range was 57.6%-121.2% and the relative standard deviation is 1.2%-11.1% when the concentration was 0.8-20 ng/L. Senventeen tap water and 30 packaged drinking water collected by the supermarket were measured. The ΣOPEs range was 16.8-177 ng/L, and the Σdi-OPEs range was 0.328-16.3 ng/L, indicating the exposure risk of organophosphates and their metabolites in water.CONCLUSION The pretreatment of the method is simple, automatic and sensitive, and is suitable for simultaneous high-throughput determination of organophosphate esters and their metabolites in large quantities of drinking water.
[1] LAO J Y,LIN H J,QIN X,et al.Insights into the atmospheric persistence,transformation,and health implications of organophosphate esters in urban ambient air[J].Environ Sci Technol,2022,56(17):12003-12013.
[2] ZHANG Z,WANG Y,TAN F,et al.Characteristics and risk assessment of organophosphorus flame retardants in urban road dust of Dalian,Northeast China[J].Sci Total Environ,2020,705:135995.
[3] WANG X,ZHU Q,YAN X,et al.A review of organophosphate flame retardants and plasticizers in the environment:analysis,occurrence and risk assessment[J].Sci Total Environ,2020,731:139071.
[4] LUO Q,GU L Y,WU Z P,et al.Distribution,source apportionment and ecological risks of organophosphate esters in surface sediments from the Liao River,Northeast China[J].Chemosphere,2020,250:126297.
[5] ZHAO L,ZHANG Y,DENG Y,et al.Traditional and emerging organophosphate esters (OPEs) in indoor dust of Nanjing,eastern China:occurrence,human exposure,and risk assessment[J].Sci Total Environ,2020,712:136494.
[6] 刘孟飞，王美，赵昂，等.超高效液相色谱-静电场轨道离子阱高分辨质谱法测定设施菜地土壤中有机磷酸二酯类化合物[J].色谱，2023,41(1):58-65.
[7] 彭凌峰，赵芳，申长鑫，等.超高效液相色谱-串联质谱法检测小龙虾中7种有机磷酸酯类阻燃剂[J].食品安全质量检测学报，2022,13(8):2405-2412.
[8] 顾俊婕，胡曼，耿阳，等.有机磷酸酯阻燃剂的人群暴露和甲状腺毒性的研究进展[J].环境化学，2022,41(1):31-45.
[9] ZHAO F,CHEN M,GAO F,et al.Organophosphorus flame retardants in pregnant women and their transfer to chorionic villi[J].Environ Sci Technol,2017,51(11):6489-6497.
[10] 侯敏敏，史亚利，蔡亚岐.液液提取-固相萃取-高效液相色谱-串联质谱测定人体血液中16种有机磷酸酯[J].色谱，2021,39(1):69-76.
[11] 李佩，曾祥英，崔君涛，等.液相色谱-串联质谱法测定尿液中7种有机磷酸酯代谢物[J].分析化学，2017,45(11):1648-1654.
[12] World Health Organization and International Programme on Chemical Safety.Flame retardants :tris(chloropropyl) phosphate and tris(2-chloroethyl) phosphate[R].Geneva:WHO,1998.
[13] MEEKER J D,STAPLETON H M.House dust concentrations of organophosphate flame retardants in relation to hormone levels and semen quality parameters[J].Environ Health Persp,2020,118(3):318-323.
[14] LEHNER A F,SAMSING F,RUMBEIHA W K.Organophosphate ester flame retardant-induced acute intoxications in dogs[J].J Med Toxicol,2010,6(4):448-458.
[15] VEEN I V D,DE BOER J.Phosphorus flame retardants:properties,production,environmental occurrence,toxicity and analysis[J].Chemosphere,2012,88(10):1119-1153.
[16] GREAVES A K,LETCHER R J.A review of organophosphate esters in the environment from biological efects to distribution and fate[J].Bull Environ Contam Tox,2017,98(1):2-7.
[17] European Commission.European Union risk assessment report:2,2-bis(chloromethyl) trimethylene bis[bis(2-chloroethyl) phosphate](V6) [R].Luxembourg:EU,2008.
[18] 许红睿，李凌，张付刚，等.膜式固相萃取-超高效液相色谱-质谱联用法测定饮用水中11种有机磷酸酯阻燃剂[J].中国卫生检验杂志，2022,32(13):1560-1563.
[19] 李洒洒，王俊霞，张占恩.超声提取-分散液液微萃取-气相色谱串联质谱法测定大气PM10中的7种有机磷酸酯阻燃剂[J].环境化学，2021,40(11):3520-3529.
[20] 张玮庭，宋善军，卢柏灵，等.加速溶剂萃取-固相萃取-层析柱净化法同时测定沉积物中多氯联苯、多溴二苯醚和有机磷阻燃剂[J].分析化学，2021,49(4):571-580.
[21] 桑永珠，厉文辉，刘杰民，等.气相色谱-质谱法测定温室大棚土壤中13种有机磷酸酯[J].分析测试学报，2020,39(12):1538-1543.
[22] 杨露敏，宋晓翠，张颖，等.自来水给水系统中有机磷酸酯的污染特征及健康风险评价[J].环境科学学报，2021,41(8):3268-3278.
[23] LI J,YU N,ZHANG B B,et al.Occurrence of organophosphate flame retardants in drinking water from China[J].Water Res,2014,54:53-61.
[24] GBADAMOSI M R,AI-OMRAN L S,ABDALLAH M A,et al.Concentrations of organophosphate esters in drinking water from the United Kingdom:implications for human exposure[J].Emergin Contam,2023,9(1):100203.
[25] DING J J,SHEN X L,LIU W P,et al.Occurrence and risk assessment of organophosphate esters in drinking water from Eastern China[J].Sci Total Environ,2015,538:959-965.
[26] PARK H J,CHOO G J,KIM H R,et al.Evaluation of the current contamination status of PFASs and OPFRs in South Korean tap water associated with its origin[J].Sci Total Environ,2018,634:1505-1512.
基本信息:
DOI：10.19813/j.cnki.weishengyanjiu.2024.01.017
中图分类号:R123.1;O657.63
引用信息:
[1]袁蕊,崔霞,佟晶,等.全自动固相萃取-液相色谱串联质谱法同时测定饮用水中21种有机磷酸酯及其代谢产物[J].卫生研究,2024,53(01):109-116+172.DOI:10.19813/j.cnki.weishengyanjiu.2024.01.017.
基金信息:
北京市东城区优秀人才培养资助项目(No.2021-dchrcprzz-44); 北京市东城区卫生科技计划项目(No.东卫健研[2023]-18)
2023-04-18
2023
2023-06-26
2023-07-03
2023
1
2024-01-17
2024-01-17