茹歌,许勇,韩晶,等.超高效液相色谱-串联质谱法测定化妆品中13种α-羟基酸[J].上海预防医学,2024,36(4):399-408.. doi: 10.19428/j.cnki.sjpm.2024.23583
引用本文: 茹歌,许勇,韩晶,等.超高效液相色谱-串联质谱法测定化妆品中13种α-羟基酸[J].上海预防医学,2024,36(4):399-408.. doi: 10.19428/j.cnki.sjpm.2024.23583
RU Ge,XU Yong,HAN Jing,et al.Determination of α-hydroxy acids in cosmetics by UHPLC-MS/MS[J].Shanghai Journal of Preventive Medicine,2024,36(04):399-408.. doi: 10.19428/j.cnki.sjpm.2024.23583
Citation: RU Ge,XU Yong,HAN Jing,et al.Determination of α-hydroxy acids in cosmetics by UHPLC-MS/MS[J].Shanghai Journal of Preventive Medicine,2024,36(04):399-408.. doi: 10.19428/j.cnki.sjpm.2024.23583

超高效液相色谱-串联质谱法测定化妆品中13α-羟基酸

Determination of α-hydroxy acids in cosmetics by UHPLC-MS/MS

  • 摘要:
    目的 建立化妆品中葡糖醛酸、酒石酸、羟基乙酸、苹果酸、乳酸、柠檬酸、2⁃羟基丁酸钠、扁桃酸、二苯乙醇酸、羟基辛酸、乳糖酸、葡糖酸、N⁃乙酰神经氨酸等13种α⁃羟基酸类化合物的超高效液相色谱⁃串联质谱(UHPLC⁃MS/MS)测定法。
    方法 水剂、膏霜、乳液类化妆品经超声提取、澄清剂净化、10 000.0 r·min-1高速离心处理,上层溶液经0.22 μm微孔滤膜过滤后进样。采用Poroshell 120 EC⁃C18反相色谱柱(2.7 μm,4.6 mm×100 mm)分离,以0.1%甲酸水溶液⁃乙腈梯度洗脱,采用电喷雾负离子源(ESI-),多反应监测(MRM)扫描方式监测,外标法定量测定。
    结果 葡糖醛酸、酒石酸、苹果酸、2⁃羟基丁酸钠、二苯乙醇酸、羟基辛酸、N⁃乙酰神经氨酸等7种化合物在50.0~2 000.0 μg·L-1的浓度范围内呈线性关系(r>0.995);羟基乙酸、乳酸、柠檬酸、扁桃酸等4种化合物在100.0~5 000.0 μg·L-1的浓度范围内呈线性关系(r>0.995);乳糖酸、葡糖酸等2种化合物在50.0~5 000.0 μg·L-1的浓度范围内呈线性关系(r>0.995)。考察了水剂、膏霜、乳液类化妆品的加标回收率。回收率结果在92.3%~114.1%,相对标准偏差(RSD)在0.9%~6.0%。葡糖醛酸、酒石酸、苹果酸、柠檬酸、2⁃羟基丁酸、二苯乙醇酸、羟基辛酸、乳糖酸、葡糖酸、N⁃乙酰神经氨酸的方法检出限均为0.003%;羟基乙酸、乳酸、扁桃酸的方法检出限均为0.006%。10批市售化妆品中8批为阳性。
    结论 UHPLC⁃MS/MS法高效、灵敏、准确,适用于化妆品中葡糖醛酸、酒石酸、羟基乙酸、苹果酸、乳酸、柠檬酸、2⁃羟基丁酸、扁桃酸、二苯乙醇酸、羟基辛酸、乳糖酸、葡糖酸、N⁃乙酰神经氨酸等13种α⁃羟基酸的检测。

     

    Abstract:
    Objective To establish a UHPLC-MS/MS quantitative method for the determination of glucuronic acid, tartaric acid, glycolic acid, malic acid, lactic acid, citric acid, DL-2-hydroxybutyric acid sodium, mandelic acid, benzilic acid, hydroxycaprylic acid, lactobionic acid, gluconic acid and N-acetylneuraminic acid in cosmetics.
    Methods Samples were prepared by ultrasonic extraction, cleansed by precipitating reagent and followed by high-speed centrifugation of the extraction solution. The supernatant was filtered by 0.22 μm Millipore filter. The continued filtrate was taken for analysis. A reversed phase column, Poroshell 120 EC-C18 (2.7 μm, 4.6 mm×1 000 mm) was used with 0.1% formic acid buffer and acetonitrile as the mobile phase under the condition of gradient elution. The analytes were detected with electrospray ionization source in negative ion mode (ESI-) and multiple reactions monitoring (MRM), and quantified by external standard curve.
    Results The method showed a good linearity of glucuronic acid, tartaric acid, malic acid, DL-2-hydroxybutyric acid sodium, benzilic acid, hydroxycaprylic acid and N-acetylneuraminic acid within the concentration range of 50.0‒2 000.0 μg·L-1r>0.995). The method showed a good linearity of glycolic acid, lactic acid, citric acid and mandelic acid within the concentration range of 100.0‒5 000.0 μg·L-1r>0.995). The method showed a good linearity of lactobionic acid and gluconic acid within the concentration range of 50.0‒5 000.0 μg·L-1r>0.995). The recoveries were in the range of 92.3%‒114.1%; the relative standard deviations (RSD) were in the range of 0.9%‒6.0% (n=3). The detection limits of glucuronic acid, tartaric acid, malic acid, citric acid, DL-2-hydroxybutyric acid sodium, mandelic acid, benzilic acid, hydroxycaprylic acid, lactobionic acid, gluconic acid and N-acetylneuraminic acid were 0.003% while the detection limits of glycolic acid, lactic acid and mandelic acid were 0.006%. In 10 batches of commercially available cosmetics, eight batches showed positive result.
    Conclusion The UHPLC-MS/MS method is efficient, sensitive and accurate and is applicable to the determination of 13 α-hydroxy acidic components in cosmetics.

     

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