目的: 建立二维柱切换高效液相色谱法测定化妆品中氢醌、苯酚的分析方法。方法: 二维色谱柱均为C18色谱柱(250 mm×4.6 mm,5 μm),捕获柱为2条串联的C16色谱柱(20 mm×4.0 mm,5 μm),10 mmol·L-1磷酸二氢钾溶液(用磷酸调节pH3.5)-甲醇为流动相,梯度洗脱,流速1.0 mL·min-1,柱温35 ℃,检测波长280 nm,进样量2 μL。结果: 氢醌和苯酚线性范围分别为5.570～111.5 μg·mL-1 (r=0.999 7)和5.410～108.1 μg·mL-1(r =0.999 6),方法提取回收率分别为91.9%~92.6%和94.4%~94.7%,精密度试验的RSD分别为3.9%~4.1%和0.9%~2.1%,检测下限分别为0.70 μg·g-1和0.69 μg·g-1。市场随机抽取40批美白类化妆品样品(包含乳剂、霜剂、水剂等)均单次进样即可快速完成样品分析,无基质干扰。结论: 本法测定美白类化妆品中氢醌、苯酚含量的专属性好,方法快速、准确,可用于复杂基质的美白类化妆品中氢醌、苯酚的测定。
Objective: To establish a method to determine hydroquinone and phenol in whitening cosmetics by switching column two-dimensional HPLC. Methods: Two C18 columns(250 mm×4.6 mm, 5 μm)and two C16 trapping columns (20 mm×4.0 mm, 5 μm)were used with the mobile phase of 10 mmol·L-1 monopotassium phosphate solution(adjusted to pH 3.5 with phosphoric acid)-methanol in a gradient elution program at a flow rate of 1 mL·min-1. The column temperature was set at 35 ℃, the determine wavelength was 280 nm, and injection volume was 2 μL. Results: Hydroquinone and phenol showed good linear relationship in the ranges of 5.570-111.5 μg·mL-1 (r=0.999 7)and 5.410-108.1 μg·mL-1(r=0.999 6). The recoveries were 91.9%-92.6% and 94.4%-94.7% with RSDs of 3.9%-4.1% and 0.9%-2.1%, respectively. Forty batches of commercially available whitening cosmetics(including emulsion, cream, astringent, etc) were analyzed by single measurement without matrix interference. Conclusion: The method has good specificity for the determination of hydroquinone and phenol in whitening cosmetics, which can determine hydroquinone and phenol in whitening cosmetics with complex matrix rapidly and accurately.
[1] 赵慧, 陈志刚, 崔岩峥, 等. 北京地区医院含苯酚制剂的风险控制[J].中国医药药学杂志, 2015, 35(9): 838
ZHAO H, CHEN ZG, CUI YZ, et al. Risk control of phenol-containing preparation in hospital in Beijing[J].Chin Hosp Pharm J, 2015, 35(9): 838
[2] 张凤兰, 苏哲, 吴景, 等. β-熊果苷和氢醌安全性评价及化妆品法规管理现状[J].环境与健杂志, 2017, 34(11): 1017
ZHANG FL, SU Z, WU J, et al. Safety assessment of beta-arbutin and hydroquinone and current situation of cosmetics regulation management[J].J Environ Health, 2017, 34(11): 1017
[3] 朱杰民, 胡静, 杜达安. 高效液相色谱法多波长测定祛斑类化妆品中氢醌和苯酚[J].环境与健康杂志, 2000, 17(2): 109
ZHU JM, HU J, DU DA. Determination of hydroquinone and phenol in freckl-removing cosmetics with multi-wavelength HPLC[J].J Environ Health, 2000, 17(2): 109
[4] 赵江丽, 张敏, 张西茹, 等. 测定美白类化妆品中氢醌和苯酚的高效液相色谱法改进研究[J].药物分析杂志, 2017, 37(3): 508
ZHAO JL, ZHANG M, ZHANG XR, et al. Improvement on determination of hydroquinone and phenol in whitening cosmetics by HPLC[J].Chin J Pharm Anal, 2017, 37(3): 508
[5] 简龙海, 袁晓倩, 郑荣, 等. 高效液相色谱-荧光检测法同时测定化妆品中的α-熊果苷、β-熊果苷、氢醌和苯酚[J].药物分析杂志, 2020, 40(2): 273
JIAN LH, YUAN XQ, ZHENG R, et al. Determination of α-arbutin, β-arbutin, hydroquinone and phenol in cosmetics by high performance liquid chromatography-fluorescent detection[J].Chin J Pharm Anal, 2020, 40(2): 273
[6] 张瑾, 王瑾, 杨英超, 等. 高效液相色谱法测定螨变应原注射液中防腐剂苯酚含量[J].药物分析杂志, 2014, 34(8): 1486
ZHANG J, WANG J, YANG YC, et al. Determination of preservative phenol in mite allergons preparation injection by HPLC[J].Chin J Pharm Anal, 2014, 34(8): 1486
[7] 朱建晖. 高效液相色谱法检测化妆品中氢醌和苯酚[J].现代预防医学, 2006, 33(5): 788
ZHU JH. Determination of hydroquinone and phenol in cosmetics with HPLC[J].Mod Prev Med, 2006, 33(5): 788
[8] 简龙海, 陈丹丹, 茹歌, 等. 高效液相色谱法同时测定化妆品中12 种美白成分[J].香料香精化妆品, 2016(6): 29
JIAN LH, CHEN DD, RU G, et al. Simultaneous determination of twelve kinds of whitening ingredients in cosmetics by high performance liquid chromatography[J].Flavour Fragrance Cosmet, 2016(6): 29
[9] 赵江丽, 康鹰, 孙菡, 等. 固相萃取-高效液相色谱法测定化妆品中氢醌和苯酚[J].中国卫生检验杂志, 2019(1): 29
ZHAO JL, KANG Y, SUN H, et al. Determination of hydroquinone and phenol in cosmetics by solid phase extraction-high performance liquid chromatography[J].Chin J Health Lab Technol, 2019(1): 29
[10] 张卫国, 郭华, 林野. 化妆品中苯酚和氢醌的气相色谱测定法[J].职业与健康, 2010, 26(1): 38
ZHANG WG, GUO H, LIN Y. Determination of phenol and hydroquinone in cosmetics by gas chromatography[J].Occup Health, 2010, 26(1): 38
[11] 陈少波, 蒲云月, 余雯静, 等. 气相色谱-质谱法测定化妆品中苯酚和氢醌[J].分析测试技术与仪器, 2017, 23(3): 176
CHEN SB, PU YY, YU WJ, et al. Determination of phenol and hydroquinone in cosmetics by gas chromatography-mass spectrometry[J].Anal Test Technol Instrum, 2017, 23(3): 176
[12] 翟宇, 尚博扬, 黄青, 等. 气相色谱-质谱法测定美白祛斑类化妆品中的苯酚和氢醌[J].宁夏医科大学学报, 2009, 41(1): 40
ZAI Y, SHANG BY, HUANG Q, et al. Determination of phenol and hydroquinone in cosmetics by gas chromatography-mass spectrometry[J].J Ningxia Med Coll, 2009, 41(1): 40
[13] 蒋珍娟, 陈志涛. β-熊果苷对GC-MS 检测化妆品中氢醌的影响[J].日用化学工业, 2017, 47(2): 118
JIANG ZJ, CHEN ZT. Influence of β-arbutin on analysis result of hydroquinone in cosmetics by GC-MS[J].China Surf Deterg Cosmet, 2017, 47(2): 118
[14] 化妆品安全技术规范 [S].2015: 302
Safety Technical Specification for Cosmetics [S].2015:302
