河北省科学院学报
河北省科學院學報
하북성과학원학보
JOURNAL OF THE HEBEI ACADEMY OF SCIENCES
2015年
1期
47-53
,共7页
周法东%张玮%李利元%卢晓宇%李强
週法東%張瑋%李利元%盧曉宇%李彊
주법동%장위%리리원%로효우%리강
化妆品%2 ,4 ,6-三氯苯酚%五氯苯酚%液相色谱-串联质谱
化妝品%2 ,4 ,6-三氯苯酚%五氯苯酚%液相色譜-串聯質譜
화장품%2 ,4 ,6-삼록분분%오록분분%액상색보-천련질보
Cosmetics%2,4,6-trichlorophenol%Pentachlorophenol%Liquid chromatography-tandem mass spectrometry
本试验建立了化妆品(爽肤水和润肤乳)中禁用的含氯苯酚(2,4,6‐三氯苯酚和五氯苯酚)的超高效液相色谱-串联质谱测定方法,采用Q1多离子监测模式。1.0g爽肤水和1.0g润肤乳样品经10 m L正己烷超声辅助提取后,取正己烷层45℃氮吹至近干,甲醇定容,经液相色谱分离、质谱测定,外标法定量。2,4,6‐三氯苯酚在添加水平200μg/kg和800μg/kg时,方法的回收率范围为81.6%-94.5%,五氯苯酚在添加水平50μg/kg和200μg/kg时回收率范围为65.3%-74.3%,相对标准偏差小于6%。爽肤水中2,4,6‐三氯苯酚和五氯苯酚的检出限分别为20μg/kg和3μg/kg ,定量限分别为50μg/kg和10μg/kg ;润肤乳中2,4,6‐三氯苯酚和五氯苯酚的检出限分别为30μg/kg和5μg/kg ,定量限分别为100μg/kg和20μg/kg。该方法可用于爽肤水和润肤乳中2,4,6‐三氯苯酚和五氯苯酚的快速筛查和定量分析。
本試驗建立瞭化妝品(爽膚水和潤膚乳)中禁用的含氯苯酚(2,4,6‐三氯苯酚和五氯苯酚)的超高效液相色譜-串聯質譜測定方法,採用Q1多離子鑑測模式。1.0g爽膚水和1.0g潤膚乳樣品經10 m L正己烷超聲輔助提取後,取正己烷層45℃氮吹至近榦,甲醇定容,經液相色譜分離、質譜測定,外標法定量。2,4,6‐三氯苯酚在添加水平200μg/kg和800μg/kg時,方法的迴收率範圍為81.6%-94.5%,五氯苯酚在添加水平50μg/kg和200μg/kg時迴收率範圍為65.3%-74.3%,相對標準偏差小于6%。爽膚水中2,4,6‐三氯苯酚和五氯苯酚的檢齣限分彆為20μg/kg和3μg/kg ,定量限分彆為50μg/kg和10μg/kg ;潤膚乳中2,4,6‐三氯苯酚和五氯苯酚的檢齣限分彆為30μg/kg和5μg/kg ,定量限分彆為100μg/kg和20μg/kg。該方法可用于爽膚水和潤膚乳中2,4,6‐三氯苯酚和五氯苯酚的快速篩查和定量分析。
본시험건립료화장품(상부수화윤부유)중금용적함록분분(2,4,6‐삼록분분화오록분분)적초고효액상색보-천련질보측정방법,채용Q1다리자감측모식。1.0g상부수화1.0g윤부유양품경10 m L정기완초성보조제취후,취정기완층45℃담취지근간,갑순정용,경액상색보분리、질보측정,외표법정량。2,4,6‐삼록분분재첨가수평200μg/kg화800μg/kg시,방법적회수솔범위위81.6%-94.5%,오록분분재첨가수평50μg/kg화200μg/kg시회수솔범위위65.3%-74.3%,상대표준편차소우6%。상부수중2,4,6‐삼록분분화오록분분적검출한분별위20μg/kg화3μg/kg ,정량한분별위50μg/kg화10μg/kg ;윤부유중2,4,6‐삼록분분화오록분분적검출한분별위30μg/kg화5μg/kg ,정량한분별위100μg/kg화20μg/kg。해방법가용우상부수화윤부유중2,4,6‐삼록분분화오록분분적쾌속사사화정량분석。
A liquid chromatography‐tandem mass spectrometry method was built to determine 2 ,4 ,6‐trichlorophenol ,pentachlorophenol in toner and moisturizer ,Q1 multiple ions scan mode was used in the experiment .1 .0 g toner and 1 .0 g moisturizer was extracted by n‐hex‐ane with ultrasonic assisted extraction .The extracts of n‐hexane were dried by nitrogen at 45℃ ,and then dissolved by methanol .Anlytes were separated by liquid chromatography ,de‐termined by mass spectrometry and quantified with external standard method .Recoveries of 2 ,4 ,6‐trichlorophenol were in range of 81 .6% -94 .5% with spike level of 200μg/kg and 800μg/kg ;recoveries of pentachlorophenol were in range of 65 .3% -74 .3% with spike level of 50μg/kg and 200μg/kg ;relative standard deviations of method w ere low er than 6% .Limit of detection of 2 , 4 , 6‐trichlorophenol and pentachlorophenol in toner was 20μg/kg 和3μg/kg ,limit of quantitation of 2 ,4 ,6‐trichlorophenol and pentachlorophenol in toner was 50μg/kg和10μg/kg ;limit of detection of 2 ,4 ,6‐trichlorophenol and pentachlorophenol in moisturizer w as 30μg/kg和5μg/kg ,limit of quantitation of 2 ,4 ,6‐trichlorophenol and pen‐tachlorophenol in moisturizer was 100μg/kg和20μg/kg .This method could be used in rapid screening and quantitative analysis of 2 ,4 ,6‐trichlorophenol ,pentachlorophenol in toner and moisturizer .