香料香精化妆品
香料香精化妝品
향료향정화장품
FLAVOUR FRAGRANCE COSMETICS
2014年
6期
39-41,46
,共4页
周耀斌%赵艳菊%周静%杨丹%杨保刚
週耀斌%趙豔菊%週靜%楊丹%楊保剛
주요빈%조염국%주정%양단%양보강
气相色谱法%壬二酸%化妆品
氣相色譜法%壬二痠%化妝品
기상색보법%임이산%화장품
gas chromatography (GC)%azelaic acid%cosmetics
采用衍生方式建立了化妆品中壬二酸的样品处理方法,确立了壬二酸衍生物的气相色谱检测方法。结果表明当衍生剂为硫酸和乙醇、衍生时间为1 h、衍生温度为70℃时,壬二酸的衍生效果比较好。采用 DB-1毛细管色谱柱,升温程序为初温80℃、20℃/min 升至300℃后保留3 min,壬二酸衍生物能够得到较好分离。用氢火焰离子化检测器检测,外标法定量。壬二酸衍生物在20~1000 mg/L 范围内线性关系良好,决定系数 r2=0.9996。气相色谱法定性检出限和定量下限分别为50.0和100.0 mg/kg,回收率为84.9%~105.8%,RSD<5%。68批次样品检测结果显示:在标称含有壬二酸的2个样品中,仅有1个检出了壬二酸,其质量比为117 mg/kg,其余67种样品均未检出壬二酸。
採用衍生方式建立瞭化妝品中壬二痠的樣品處理方法,確立瞭壬二痠衍生物的氣相色譜檢測方法。結果錶明噹衍生劑為硫痠和乙醇、衍生時間為1 h、衍生溫度為70℃時,壬二痠的衍生效果比較好。採用 DB-1毛細管色譜柱,升溫程序為初溫80℃、20℃/min 升至300℃後保留3 min,壬二痠衍生物能夠得到較好分離。用氫火燄離子化檢測器檢測,外標法定量。壬二痠衍生物在20~1000 mg/L 範圍內線性關繫良好,決定繫數 r2=0.9996。氣相色譜法定性檢齣限和定量下限分彆為50.0和100.0 mg/kg,迴收率為84.9%~105.8%,RSD<5%。68批次樣品檢測結果顯示:在標稱含有壬二痠的2箇樣品中,僅有1箇檢齣瞭壬二痠,其質量比為117 mg/kg,其餘67種樣品均未檢齣壬二痠。
채용연생방식건립료화장품중임이산적양품처리방법,학립료임이산연생물적기상색보검측방법。결과표명당연생제위류산화을순、연생시간위1 h、연생온도위70℃시,임이산적연생효과비교호。채용 DB-1모세관색보주,승온정서위초온80℃、20℃/min 승지300℃후보류3 min,임이산연생물능구득도교호분리。용경화염리자화검측기검측,외표법정량。임이산연생물재20~1000 mg/L 범위내선성관계량호,결정계수 r2=0.9996。기상색보법정성검출한화정량하한분별위50.0화100.0 mg/kg,회수솔위84.9%~105.8%,RSD<5%。68비차양품검측결과현시:재표칭함유임이산적2개양품중,부유1개검출료임이산,기질량비위117 mg/kg,기여67충양품균미검출임이산。
In this study,a gas chromatography method for the determination of azelaic acid in cosmetics was established in de-rivative way.The results showed that when the derivative agent were sulfuric acid and ethanol,derivative time was 1 h,tem-perature was 70 ℃,the derivative effect was good.By using DB-1 capillary column,when the temperature program was as fol-lows:the initial temperature 80 ℃,at rate of 20 ℃/min to 300 ℃,the retention time 3 min,the azelaic acid derivatives could be well separated.The hydrogen flame ionization detector was used and azelaic acid was quantified by external standard meth-od.In the range of 20 to 1 000 mg/L,the linear relationship of azelaic acid derivatives were good,the correlation coefficient r2=0.9996,qualitative detection limit was 50.0 mg/kg,quantitative limit was 100 mg/kg.The recovery rate was 84.9% to 105.8%,RSD<5%.The test results of 68 batches of samples showed that only one was detected among 2 samples claimed containing azelaic acid,and its mass ratio was 117 mg/kg,the other 67 samples were no azelaic acid detected.