高效液相色谱法测定润肤霜和洗发露中的银杏黄酮类物质

Determination of ginkgo glycosides in cream and shampoo products by high performance liquid chromatography

建立了测定润肤霜和洗发露中3种银杏黄酮类物质（槲皮素、山萘素和异鼠李素）的高效液相色谱分析方法。样品经甲醇提取、离心后，提取液以FortisPhenyl色谱柱（4．6×250mm，5μm）分离，体积分数0．5％H3PO4-甲醇流动相体系等度洗脱，在波长367nm下用二极管阵列检测器检测，以保留时间结合紫外光谱定性，外标法定量。结果表明：3种目标分析物分离度好；在0．25—50．0mg／L范围内线性关系良好，相关系数为0．9992—0．9999；槲皮素、山萘素和异鼠李素的方法检出限（s／N=3）分别为0．8，1．0和1．0mg／kg；添加水平为5～500mg／kg时，回收率为83．5％-102．8％，相对标准偏差（RSD，n=6）为1．6％-6．5％。方法适用于护肤类和洗护发类化妆品中槲皮素、山萘素和异鼠李素的测定。

A new efficient method was established for the first time to determine Ginkgo kaempferol and isorhamnetin） in cream and shampoo products by high performance liquid glycosides （ quercetin, chromatography with a diode array detector （HPLC-DAD）. Samples were extracted with methanol, centrifugated, separated on a Fortis Phenyl column （4. 6 ×250mm,5μm）, eluted with methanol - 0. 5% phosphoric acid, and analyzed by HPLC-DAD at 367 nm. The targets were qualitatively determined by retention time combined with ultraviolet spectrum confirmation, and additionally quantitatively determined by external standard methods. The main factors affecting the methodology development including the extraction procedure, the elution solvent, and the chromatographic column were assessed and optimized through a multi-categorical experimental design, using a real cosmetic sample. Under the optimal conditions, it showed satisfactory linearity, repeatability and intermediate precision. In the ranging of 0. 25 ~ 50 mg/L, the target analytes showed good linearity with correlation coefficient （r） ranging from 0. 9992 to 0. 9999. The detection limits of quercetin, kaempferol and isorhamnetin （S/N = 3） were 0. 8, 1.0 and 1.0 mg/kg, respectively. At the spiking levels of 5 - 500 mg/kg, satisfactory recoveries ranged from 83.5% to 102%. In all cases, the method precision （RSD, n = 6） were between 1.6% and 6. 5%, which makes this low cost extraction method reliable for routine analysis. The validated method was successfully utilized to determine the Ginkgo glycosides in real cosmetics without the need for tedious pretreatments. The results showed that this method was stable, accurate and precise, and it showed potential application in the analysis of the three mentioned compounds in skin care and hair care oroduets.