分析化学
分析化學
분석화학
CHINESE JOURNAL OF ANALYTICAL CHEMISTRY
2009年
12期
1776-1780
,共5页
马强%白桦%王超%马微%张庆%肖海清%周新%董益阳%王宝麟
馬彊%白樺%王超%馬微%張慶%肖海清%週新%董益暘%王寶麟
마강%백화%왕초%마미%장경%초해청%주신%동익양%왕보린
固相萃取%同位素稀释%气相色谱-串联质谱%化妆品%二甲苯麝香
固相萃取%同位素稀釋%氣相色譜-串聯質譜%化妝品%二甲苯麝香
고상췌취%동위소희석%기상색보-천련질보%화장품%이갑분사향
Solid phase extraction%isotope dilution%gas chromatography tandem mass spectrometry%cosmetics%musk xylene
建立了测定化妆品中二甲苯麝香的固相萃取-同位素稀释-气相色谱-串联质谱分析方法.膏霜、水剂、散粉、香波、唇膏等不同类型的化妆品样品加入甲醇经超声提取后,样品提取液高速离心处理,浓缩上清液,以Sep-Pak Silica固相萃取柱净化,收集二氯甲烷洗脱液,DB-5 MS(30 m × 0.25 mm, 0.25 μm)石英毛细管色谱柱分离后经NCI-GC-MS/MS多反应监测技术进行定性及定量分析.二甲苯麝香的方法定量限为5 μg/kg,在5～50 μg/kg范围内的3个添加水平的平均回收率为81.1%～86.9%,日内精密度均小于10%,日间精密度均小于12%.本方法准确、快速、灵敏度高,可用于化妆品的实际检验工作.
建立瞭測定化妝品中二甲苯麝香的固相萃取-同位素稀釋-氣相色譜-串聯質譜分析方法.膏霜、水劑、散粉、香波、脣膏等不同類型的化妝品樣品加入甲醇經超聲提取後,樣品提取液高速離心處理,濃縮上清液,以Sep-Pak Silica固相萃取柱淨化,收集二氯甲烷洗脫液,DB-5 MS(30 m × 0.25 mm, 0.25 μm)石英毛細管色譜柱分離後經NCI-GC-MS/MS多反應鑑測技術進行定性及定量分析.二甲苯麝香的方法定量限為5 μg/kg,在5～50 μg/kg範圍內的3箇添加水平的平均迴收率為81.1%～86.9%,日內精密度均小于10%,日間精密度均小于12%.本方法準確、快速、靈敏度高,可用于化妝品的實際檢驗工作.
건립료측정화장품중이갑분사향적고상췌취-동위소희석-기상색보-천련질보분석방법.고상、수제、산분、향파、진고등불동류형적화장품양품가입갑순경초성제취후,양품제취액고속리심처리,농축상청액,이Sep-Pak Silica고상췌취주정화,수집이록갑완세탈액,DB-5 MS(30 m × 0.25 mm, 0.25 μm)석영모세관색보주분리후경NCI-GC-MS/MS다반응감측기술진행정성급정량분석.이갑분사향적방법정량한위5 μg/kg,재5～50 μg/kg범위내적3개첨가수평적평균회수솔위81.1%～86.9%,일내정밀도균소우10%,일간정밀도균소우12%.본방법준학、쾌속、령민도고,가용우화장품적실제검험공작.
A comprehensive analytical method based on solid phase extraction-isotope dilution-gas chromatography tandem mass spectrometry has been developed for the determination of musk xylene in cosmetics. Various cosmetic samples, including cream, lotion, powder, shampoo and lipstick, were extracted under ultrasonication. The extract was centrifuged, and the upper solution was concentrated by rotary evaporator. The reconstructed solution was then cleaned up by Sep-Pak Silica solid phase extraction cartridge. Qualitative and quantitative analysis was carried out under the MRM mode after the chromatographic separation on DB-5 MS(30 m×0.25 mm, 0.25 μm) capillary column. The limit of quantitation(LOQ) for musk xylene was 5 μg/kg. The mean recoveries at the three spiked levels of 5-50 μg/kg were 81.1%-86.9%, with the intra-day precision less than 10% and the inter-day precision less than 12%. The method is accurate, rapid, sensitive and adapt to the inspection of musk xylene in cosmetics.
