高效液相色譜-串聯(lián)質(zhì)譜法測定泡沫滅火材料及其他材料中的全氟辛烷磺酸及其鹽

陳會明, 程 艷, 陳 偉, 于文蓮, 李 晞, 王 琤

(國家質(zhì)量監(jiān)督檢驗(yàn)檢疫總局進(jìn)出口化學(xué)品安全研究中心,中國檢驗(yàn)檢疫科學(xué)研究院,北京100123)

高效液相色譜-串聯(lián)質(zhì)譜法測定泡沫滅火材料及其他材料中的全氟辛烷磺酸及其鹽

陳會明＊, 程 艷, 陳 偉, 于文蓮, 李 晞, 王 琤

(國家質(zhì)量監(jiān)督檢驗(yàn)檢疫總局進(jìn)出口化學(xué)品安全研究中心,中國檢驗(yàn)檢疫科學(xué)研究院,北京100123)

建立了一種高效液相色譜-串聯(lián)質(zhì)譜(HPLC-MS/MS)測定泡沫滅火材料、洗滌劑以及織物整理劑中全氟辛烷磺酸及其鹽(PFOS)的方法。對應(yīng)產(chǎn)品中的PFOS用水超聲提取后,經(jīng)固相萃取柱淋洗萃取,萃取液以乙腈-10 mmol/L乙酸銨溶液(80∶20,v/v)為流動相進(jìn)行HPLC分離,在負(fù)離子模式和多級反應(yīng)監(jiān)測(MRM)方式下進(jìn)行測定。用兩個(gè)子離子的相對豐度定性,外標(biāo)法定量。PFOS的測定在0.002～0.1m g/L范圍內(nèi)線性關(guān)系良好(r2=0.998);泡沫滅火材料、洗滌劑以及織物整理劑中PFOS的加標(biāo)回收率分別為93.4%～103%,93.2%～102%和91.8%～102%,精密度(以相對標(biāo)準(zhǔn)偏差(RSD)計(jì))分別為0.48%～3.52%,0.78%～1.79%和0.47%～3.47%;方法的檢出限均為2m g/kg(0.000 2%)(信噪比(S/N)≥10),滿足歐盟法規(guī)對泡沫滅火材料、洗滌劑以及織物整理劑中PFOS的限量檢測要求。該方法準(zhǔn)確度和靈敏度高,前處理簡單,可用于泡沫滅火材料、洗滌劑以及織物整理劑中PFOS的檢測。

高效液相色譜-串聯(lián)質(zhì)譜法(HPLC-MS/MS);固相萃取;全氟辛烷磺酰基化合物(PFOS);泡沫滅火材料;洗滌劑;織物整理劑

Abstract:A novel method based on high performance liquid Chromatography-tandem mass spectrometry(HPLC-MS/MS)was developed for the determination of perfluorooctane sulfonates(PFOS)in the fire-fighting foam,detergents and fabric finishing agents.The PFOS residue was extracted with water at first by ultrasonic,then separated by high-speed centrifugation.The supernatant was purified by p re-conditioned solid phase extraction(SPE)micro-column,and the extract was filtrated through a membrane with 0.2μm diameter.The filtrated liquid was analyzed by HPLC using acetonitrile-10mmol/L ammonium acetate solution(80∶20,v/v)as mobile phase.The PFOS was detected by using negative electrospray ionization(ESI)on a tandem mass spectrometer in multiple reaction monitoring(MRM)m ode.The qualitative analysis of the PFOS can be perform ed by using the relative abundance of two daughter ions of PFOS,and the quantitative analysis was perform ed by external standard method.The linear calibration curve was obtained in the range of0.002-0.1m g/L with a linear correlation coefficient(r2)of0.998.The spiked recoveries for PFOS in the fire-fighting foam,detergents and fabric finishing agents were93.4%-103%,93.2%-102%and91.8%-102%with the relativestandard deviation of0.48%-3.52%,0.78%-1.79%and0.47%-3.47%,respectively.And the detection limit for PFOS was2m g/kg(S/N≥10),which can meet the requirement for the PFOS restriction in fire-fighting foam,detergents and fabric finishing agents in the EU directives.with high accuracy and sensitivity,the method is simple and rap id,and can be used for PFOS inspection in fire-fighting foam,detergents and fabric finishing agents.

Key words:high performance liquid Chromatography-tandem mass spectrometry(HPLC-MS/MS);solid phase extraction(SPE);perfluorooctane sulfonates(PFOS);fire-fighting foam;detergents;fabric finishing agents

全氟辛烷磺酸及其鹽(perfluorooctane sulfonate,PFOS)是一類重要的全氟表面活性劑,因?yàn)槠涮厥獾氖杷⑹栌秃涂刮勰芰Χ鳛榉浪⒎烙汀⒎牢厶幚韯┑闹饕煞?廣泛應(yīng)用在近千種不同的民用和工業(yè)產(chǎn)品,如滅火材料、洗滌劑、織物整理劑、涂料、食品包裝材料、不粘炊具、皮革制品等生產(chǎn)中。……