CAJ | 학술논문

建立了一种反相高效液相色谱同时测定防晒类化妆品中15种紫外线吸收剂的分析方法。化妆水、乳液、膏霜和蜡质样品中首先加入四氢呋喃（含2g／L氢氧化铵），涡旋、振荡、混匀（若蜡质样品仍分散不完全，可超声振荡加热至50℃），再加入80％（v／v）甲醇水溶液振荡混匀、超声提取、离心、过滤后，采用 XTerra MS C18柱分离，经水（含0.1％（v／v）甲酸）和甲醇（含0.1％（v／v）甲酸）梯度洗脱，以二极管阵列检测器检测，检测波长为280 nm 和311 nm，外标法定量。实验中对不同基质类型样品的前处理条件（样品分散溶剂、萃取溶剂和萃取时间等）进行了重点优化。结果表明，15种紫外线吸收剂在各自的线性范围内呈良好的线性关系（ r2≥0.9991），方法的定量限为1.2~5.1 μg／g，在低、中、高3个添加水平下的回收率为84.2％~100.7％，相对标准偏差（ RSD）为0.9％~9.5％。该分析方法分离效果好、灵敏度高、定量准确，可用于防晒类化妆品的实际检测。
건립료일충반상고효액상색보동시측정방쇄류화장품중15충자외선흡수제적분석방법。화장수、유액、고상화사질양품중수선가입사경부남（함2g／L경양화안），와선、진탕、혼균（약사질양품잉분산불완전，가초성진탕가열지50℃），재가입80％（v／v）갑순수용액진탕혼균、초성제취、리심、과려후，채용 XTerra MS C18주분리，경수（함0.1％（v／v）갑산）화갑순（함0.1％（v／v）갑산）제도세탈，이이겁관진렬검측기검측，검측파장위280 nm 화311 nm，외표법정량。실험중대불동기질류형양품적전처리조건（양품분산용제、췌취용제화췌취시간등）진행료중점우화。결과표명，15충자외선흡수제재각자적선성범위내정량호적선성관계（ r2≥0.9991），방법적정량한위1.2~5.1 μg／g，재저、중、고3개첨가수평하적회수솔위84.2％~100.7％，상대표준편차（ RSD）위0.9％~9.5％。해분석방법분리효과호、령민도고、정량준학，가용우방쇄류화장품적실제검측。
An analytical method for the simultaneous determination of fifteen ultraviolet( UV) filters in sunscreen cosmetics was developed by high performance liquid chromatography ( HPLC ). Various cosmetic samples including lotions, emulsions, creams and waxes were firstly mixed thoroughly by adding tetrahydrofuran containing 2 g/L ammonium hydroxide followed by vortex and oscillation. If the wax samples were still homogenized incompletely,a ultrasonic oscillation protocol with heating to 50 ℃ was adopted. The homogeneous samples were then ultrasonically extracted by 80% aqueous methanol solution. After centrifugation and micropore filtration,the extracted components were separated on an XTerra MS C 18 column with gradient elution by water containing 0. 1%( v/v ) formic acid and methanol containing 0. 1%( v/v)formic acid,determined by a diode array detector( DAD)at 280 nm and 311 nm, and quantified using external standard method. Optimization for the pretreatment conditions of different matrices of cosmetics including sample dispersion solvents,extraction solvents and time were carried out. This developed method showed good linearity( r2≥0. 999 1)and the limits of quantification( LOQs)were between 1. 2 and 5. 1 μg/g. The recoveries of the fifteen compounds ranged from 84. 2% to 100. 7% at three spiked levels with the relative standard devi-ations( RSDs)between 0. 9% and 9. 5%. The analytes were well separated and this analytical method proved to be sensitive and accurate,so it can be used in the practical determination of the fifteen UV filters in commercial sunscreen cosmetics.