Kim Kicheol, Mueller Jochen, Park Yong-Bae, Jung Hong-Rae, Kang Seok-Ho, Yoon Mi-Hye, Lee Jeung-Bok
Gyeonggi-do Institute of Health and Environment, 324-1 Pajang-Dong, Jangan-Gu, Suwon, Gyeonggi-Do 440-290, South Korea.
J Chromatogr Sci. 2011 Aug;49(7):554-9. doi: 10.1093/chrsci/49.7.554.
HPLC method for quantitative determination of four preservatives and nine UV filters worldwide authorized in commercial suncare product was developed and validated, and then 101 samples of commercial suncare products were analyzed for the UV filters and preservatives using the proposed method. The mobile phase was acetonitrile-water containing 0.5% acetic acid using a gradient elution at a flow rate of 0.9 mL/min and UV measurements were carried out at 320 nm for UV filters and 254 nm for preservatives. The correlation coefficients of each calibration curves were mostly higher than 0.999. The percent relative standard deviations (%RSD) ranged from 0.97% to 6.1% for five sample aliquots. The recoveries from the spiked solutions were 98-102%. 2-ethylhexyl-p-methoxycinnamate (EHMC) was detected in 96 of 101 commercial suncare products and the concentration was in the range of 3.08-8.16% and 18 samples were found to exceed the 7.5% which has been defined as the maximum allowed concentration in Korea. Methyl paraben was detected in 81 of 101 samples and the next-most often detected preservatives were propyl paraben (25), ethyl paraben (18), and butyl paraben (4). Three samples of 101 suncare products exceeded the maximum allowed concentration (i.e., 0.58-0.79%). The proposed HPLC method allows efficient and simultaneous analysis of preservatives and UV filters suitable for quality control assays of commercial suncare products.
建立并验证了用于定量测定全球商业防晒产品中四种防腐剂和九种紫外线过滤剂的高效液相色谱法（HPLC），然后使用该方法对101份商业防晒产品样品中的紫外线过滤剂和防腐剂进行了分析。流动相为含0.5%乙酸的乙腈-水，采用梯度洗脱，流速为0.9 mL/min，紫外线过滤剂在320 nm处进行紫外测定，防腐剂在254 nm处进行测定。各校准曲线的相关系数大多高于0.999。五个样品等分试样的相对标准偏差百分比（%RSD）范围为0.97%至6.1%。加标溶液的回收率为98 - 102%。在101份商业防晒产品中的96份中检测到了2-乙基己基对甲氧基肉桂酸酯（EHMC），其浓度范围为3.08 - 8.16%，发现有18个样品超过了韩国规定的7.5%的最大允许浓度。在101个样品中的81个中检测到了对羟基苯甲酸甲酯，其次最常检测到的防腐剂是对羟基苯甲酸丙酯（25个）、对羟基苯甲酸乙酯（18个）和对羟基苯甲酸丁酯（4个）。101份防晒产品中的三个样品超过了最大允许浓度（即0.58 - 0.79%）。所提出的HPLC方法能够高效、同时分析防腐剂和紫外线过滤剂，适用于商业防晒产品的质量控制检测。
