分析化学
分析化學
분석화학
CHINESE JOURNAL OF ANALYTICAL CHEMISTRY
2010年
2期
197-201
,共5页
马强%白桦%王超%张庆%周新%董辉%王宝麟
馬彊%白樺%王超%張慶%週新%董輝%王寶麟
마강%백화%왕초%장경%주신%동휘%왕보린
加速溶剂萃取%固相萃取%液相色谱-串联质谱%纺织品%食品包装材料%壬基酚%辛基酚%双酚A
加速溶劑萃取%固相萃取%液相色譜-串聯質譜%紡織品%食品包裝材料%壬基酚%辛基酚%雙酚A
가속용제췌취%고상췌취%액상색보-천련질보%방직품%식품포장재료%임기분%신기분%쌍분A
Accelerated solvent extraction%Solid phase extraction%Liquid chromatography tandem mass spectrometry)%Textiles%Food packaging materials%Nonylphenols%Octylphenols%Bisphenol A
建立了纺织品和食品包装材料中壬基酚、辛基酚和双酚A的液相色谱-串联质谱分析方法.不同类型的纺织品和食品包装材料样品采用加速溶剂萃取法,以无水乙醇为提取剂,在10.3 MPa和120 ℃下静态循环提取2次,提取液经Supelclean Envi-Carb石墨化碳黑固相萃取柱净化,收集甲醇-二氯甲烷(1∶ 4, V/V)洗脱液,采用Waters XBridge C_(18))色谱柱,以甲醇-0.1%氨水溶液为流动相,梯度洗脱分离后,在LC/MS/MS多反应监测模式下进行定性与定量分析.壬基酚、辛基酚和双酚A的方法检出限为0.5 μg/kg,在0.5~10 μg/kg的3个添加水平范围内,纺织品样品的平均回收率为86.9%~92.5%,相对标准偏差均小于9.1%;食品包装材料样品的平均回收率为87.8%~93.0%,相对标准偏差均小于8.8%.本方法准确、快速、灵敏度高,可用于纺织品和食品包装材料的实际检验.
建立瞭紡織品和食品包裝材料中壬基酚、辛基酚和雙酚A的液相色譜-串聯質譜分析方法.不同類型的紡織品和食品包裝材料樣品採用加速溶劑萃取法,以無水乙醇為提取劑,在10.3 MPa和120 ℃下靜態循環提取2次,提取液經Supelclean Envi-Carb石墨化碳黑固相萃取柱淨化,收集甲醇-二氯甲烷(1∶ 4, V/V)洗脫液,採用Waters XBridge C_(18))色譜柱,以甲醇-0.1%氨水溶液為流動相,梯度洗脫分離後,在LC/MS/MS多反應鑑測模式下進行定性與定量分析.壬基酚、辛基酚和雙酚A的方法檢齣限為0.5 μg/kg,在0.5~10 μg/kg的3箇添加水平範圍內,紡織品樣品的平均迴收率為86.9%~92.5%,相對標準偏差均小于9.1%;食品包裝材料樣品的平均迴收率為87.8%~93.0%,相對標準偏差均小于8.8%.本方法準確、快速、靈敏度高,可用于紡織品和食品包裝材料的實際檢驗.
건립료방직품화식품포장재료중임기분、신기분화쌍분A적액상색보-천련질보분석방법.불동류형적방직품화식품포장재료양품채용가속용제췌취법,이무수을순위제취제,재10.3 MPa화120 ℃하정태순배제취2차,제취액경Supelclean Envi-Carb석묵화탄흑고상췌취주정화,수집갑순-이록갑완(1∶ 4, V/V)세탈액,채용Waters XBridge C_(18))색보주,이갑순-0.1%안수용액위류동상,제도세탈분리후,재LC/MS/MS다반응감측모식하진행정성여정량분석.임기분、신기분화쌍분A적방법검출한위0.5 μg/kg,재0.5~10 μg/kg적3개첨가수평범위내,방직품양품적평균회수솔위86.9%~92.5%,상대표준편차균소우9.1%;식품포장재료양품적평균회수솔위87.8%~93.0%,상대표준편차균소우8.8%.본방법준학、쾌속、령민도고,가용우방직품화식품포장재료적실제검험.
A comprehensive analytical method based on liquid chromatography tandem mass spectrometry has been developed for the determination of nonylphenol, octylphenol and bisphenol A in textiles and food packaging) materials. Various textile and food packaging material samples were extracted under the conditions of 10.3 MPa and 120 ℃ by accelerated solvent extraction method with two static cycles using ethanol as the extraction) solvent. The extract was cleaned up by Supelclean Envi-Carb solid phase extraction cartridge. Qualitative) and quantitative analyses were carried out for the analytes under the multiple reaction monitoring(MRM) mode after the chromatographic separation on Waters XBridge C_(18))(150 mm×2.1 mm, 3.5 μm) column) with methanol-0.1% NH_4OH gradient elution. The limits of detection(LODs) for alkylphenol, octyphenol and bisphenol A were 0.5 μg/kg. The mean recoveries for textile samples at the spiked level of 0.5-10 μg/kg were 86.9%-92.5%, with the relative standard deviation less than 9.1%. The mean recoveries for food packaging material samples at the spiked level of 0.5-10 μg/kg were 87.8%-93.0%, with the relative standard deviation less than 8.8%. The method is accurate, simple, rapid, and adapts to the inspection of nonylphenol, octylphenol and bisphenol A in textiles and food packaging materials.