色谱
色譜
색보
Chinese Journal of Chromatography
2015年
11期
1186-1191
,共6页
赖晓芳%冯岸红%幸苑娜%叶淋泉%林志惠%陈泽勇
賴曉芳%馮岸紅%倖苑娜%葉淋泉%林誌惠%陳澤勇
뢰효방%풍안홍%행원나%협림천%림지혜%진택용
固相萃取%气相色谱/质谱法%有机磷酸酯阻燃剂%儿童手推车
固相萃取%氣相色譜/質譜法%有機燐痠酯阻燃劑%兒童手推車
고상췌취%기상색보/질보법%유궤린산지조연제%인동수추차
solid phase extraction( SPE)%gas chromatography-mass spectrometry( GC-MS)%organophosphate ester( OPE)flame retardants%baby carriages
有机磷酸酯是一类重要的磷系阻燃剂,由于其具有类似持久性有机污染物( persistent organic pollutants, POPs)的性质,欧美等国家已纷纷设立相关法规限制其在儿童用品中的使用。目前国际和国内均未有儿童手推车中有机磷酸酯阻燃剂的检测标准。本文建立了儿童手推车中3种有机磷酸酯阻燃剂的超声萃取-弗罗里硅土固相萃取柱净化-气相色谱/质谱检测方法。该方法的加标回收率为89.5%~107.3%,检出限(3S/N)为0.01 mg/kg,定量限(10S/N)为0.1 mg/kg,能较好地排除基质干扰,适用于儿童手推车软垫材料中3种有机磷酸酯的定性和定量分析。37个样品的分析结果表明,磷酸三(2-氯丙基)酯( TCPP )的检出率为81.1%,含量范围为1.0~15312.8 mg/kg,依据欧盟玩具新指令2014/79/EU,TCPP超标(>5 mg/kg)率为32.4%;其中2个样品中还检出了磷酸三(2-氯乙基)酯(TCEP)和磷酸三(1,3-二氯-2-丙基)酯(TDCP),含量范围为6.2~44.1 mg/kg,均已超标。可见,市场上的儿童手推车存在较高的有机磷酸酯阻燃剂暴露风险。
有機燐痠酯是一類重要的燐繫阻燃劑,由于其具有類似持久性有機汙染物( persistent organic pollutants, POPs)的性質,歐美等國傢已紛紛設立相關法規限製其在兒童用品中的使用。目前國際和國內均未有兒童手推車中有機燐痠酯阻燃劑的檢測標準。本文建立瞭兒童手推車中3種有機燐痠酯阻燃劑的超聲萃取-弗囉裏硅土固相萃取柱淨化-氣相色譜/質譜檢測方法。該方法的加標迴收率為89.5%~107.3%,檢齣限(3S/N)為0.01 mg/kg,定量限(10S/N)為0.1 mg/kg,能較好地排除基質榦擾,適用于兒童手推車軟墊材料中3種有機燐痠酯的定性和定量分析。37箇樣品的分析結果錶明,燐痠三(2-氯丙基)酯( TCPP )的檢齣率為81.1%,含量範圍為1.0~15312.8 mg/kg,依據歐盟玩具新指令2014/79/EU,TCPP超標(>5 mg/kg)率為32.4%;其中2箇樣品中還檢齣瞭燐痠三(2-氯乙基)酯(TCEP)和燐痠三(1,3-二氯-2-丙基)酯(TDCP),含量範圍為6.2~44.1 mg/kg,均已超標。可見,市場上的兒童手推車存在較高的有機燐痠酯阻燃劑暴露風險。
유궤린산지시일류중요적린계조연제,유우기구유유사지구성유궤오염물( persistent organic pollutants, POPs)적성질,구미등국가이분분설립상관법규한제기재인동용품중적사용。목전국제화국내균미유인동수추차중유궤린산지조연제적검측표준。본문건립료인동수추차중3충유궤린산지조연제적초성췌취-불라리규토고상췌취주정화-기상색보/질보검측방법。해방법적가표회수솔위89.5%~107.3%,검출한(3S/N)위0.01 mg/kg,정량한(10S/N)위0.1 mg/kg,능교호지배제기질간우,괄용우인동수추차연점재료중3충유궤린산지적정성화정량분석。37개양품적분석결과표명,린산삼(2-록병기)지( TCPP )적검출솔위81.1%,함량범위위1.0~15312.8 mg/kg,의거구맹완구신지령2014/79/EU,TCPP초표(>5 mg/kg)솔위32.4%;기중2개양품중환검출료린산삼(2-록을기)지(TCEP)화린산삼(1,3-이록-2-병기)지(TDCP),함량범위위6.2~44.1 mg/kg,균이초표。가견,시장상적인동수추차존재교고적유궤린산지조연제폭로풍험。
Organophosphate esters ( OPEs ) are high-production-volume chemicals used as flame retardants. Some western countries( e. g. America and European Union)have imposed restrictions on OPEs in baby products due to their similar persistent-organic-pollutants( POPs) properties. So far,there is no domestic or foreign standard for OPEs flame retardants in baby carriages. Ultrasonic extraction was used to extract three OPEs from baby carriages,and the extracts were purified by a florisil solid phase extraction( SPE)column,and finally detected by gas chromatography-mass spectrometry( GC-MS). The spiked recoveries of the three OPEs were in the range of 89. 5% to 107. 3%. The limits of detection(3S/N)were 0. 01 mg/kg,and the limits of quantification ( 10S/N ) were 0. 1 mg/kg. This method could eliminate matrix effects and give accurate qualitative analytical results for the three OPE flame retardants in baby carriages. Thirty-seven samples were analyzed and the tris( 2-chloro-1-methylethyl)phosphate ( TCPP)detection rate was up to 81. 1% with the mass concentration range of 1. 0-15 312. 8 mg/kg,and 32. 4% of the samples exceeded the European Union directive( 2014/79/EU )for TCPP(>5 mg/kg),as well as tris(2-chloroethyl)phosphate(TCEP)and tris[2-chloro-1-( chloromethyl)ethyl]phosphate( TDCP)in two samples,which were in the range of 6. 2-44. 1 mg/kg. Thus,relatively high OPEs flame retardants risk was presented in baby carriages.