Chen Lijian, Huang Jinfeng, He Minheng, Lin Senyu, Guo Xindong
Guangzhou Quality Supervision and Testing Institute, Guangzhou 510110, China.
Se Pu. 2012 Jun;30(6):630-4. doi: 10.3724/sp.j.1123.2012.02015.
A novel analytical method for the simultaneous determination of seven naphthalenediols (2,6-naphthalenediol, 1,5-naphthalenediol, 1,6-naphthalenediol, 2,7-naphthalenediol, 1,7-naphthalenediol, 1,3-naphthalenediol and 2,3-naphthalenediol) in cosmetics by reversed-phase high performance liquid chromatography (RP-HPLC) with a diode array detector was established. The moisturizer, cream, emulsion and water-like cosmetic samples were extracted with 95% ethanol (v/v), and the powder-like cosmetic samples were extracted with 95% ethanol-0.1% acetic acid (3: 2, v/v), then the extracts were centrifuged, filtrated, and analyzed by RP-HPLC using a C18 column, employing methanol-0.1% acetic acid aqueous solution as the mobile phases under the condition of gradient elution. The naphthalenediols were qualitatively determined by retention times, and confirmed by ultraviolet spectra. The external standard method was applied for the quantification. The results indicated that the limits of quantification (LOQs) of the seven naphthalenediols were ranged from 0.5 mg/kg to 1.2 mg/kg (S/N = 10); meanwhile, the linear correlation coefficients of them were all no less than 0.999 0 within the linear ranges. Their recoveries in spiked samples at the levels of 5.0 - 50 mg/kg were ranged from 84.0% to 102% with the relative standard deviations (RSDs) of 1.3% - 5.7% (n = 6). The method is simple, precise and suitable for the determination of naphthalenediols in cosmetic samples.
建立了一种采用二极管阵列检测器的反相高效液相色谱(RP-HPLC)同时测定化妆品中七种萘二醇(2,6-萘二醇、1,5-萘二醇、1,6-萘二醇、2,7-萘二醇、1,7-萘二醇、1,3-萘二醇和2,3-萘二醇)的新型分析方法。保湿霜、乳膏、乳液和水样化妆品样品用95%乙醇(v/v)萃取,粉状化妆品样品用95%乙醇-0.1%乙酸(3:2,v/v)萃取,然后将萃取液离心、过滤,采用C18柱通过RP-HPLC分析,以甲醇-0.1%乙酸水溶液为流动相进行梯度洗脱。通过保留时间对萘二醇进行定性测定,并通过紫外光谱进行确认。采用外标法进行定量。结果表明,七种萘二醇的定量限(LOQ)为0.5 mg/kg至1.2 mg/kg(S/N = 10);同时,它们在各自线性范围内的线性相关系数均不小于0.999 0。在加标水平为5.0 - 50 mg/kg的样品中,其回收率为84.0%至102%,相对标准偏差(RSD)为1.3% - 5.7%(n = 6)。该方法简便、准确,适用于化妆品样品中萘二醇的测定。