Significant developments have recently been achieved in the field of N-lauryl amino acid (NLAA) surfactants derived from renewable resources. Compared with conventional surfactants, NLAAs exhibit remarkable surfactant properties, exceptional biodegradability, good biocompatibility, and high safety profiles. These attributes have led to the widespread use of NLAAs in personal-care products. The detection methods employed for NLAAs include two-phase titration (TT), spectrophotometric analysis (SA), and high performance liquid chromatography (HPLC). However, because both TT and SA measure the total concentration of anionic active matter, identifying and quantifying individual compounds in a sample containing multiple anionic surfactants is impossible. The presence of cationic surfactants in the sample also introduces interferences, which lead to significant errors. Compared with TT and SA, HPLC offers direct and rapid testing procedures. However, compounds with no or weak UV-visible light absorption exhibit low sensitivity when detected by UV, necessitating the use of detectors such as differential refractive index detectors (RIDs), evaporative light scattering detectors (ELSDs), or charged aerosol detectors (CADs). Most HPLC users consider UV light as the fundamental configuration of the instrument, and other detectors are less commonly employed. Therefore, establishing a new HPLC method suitable for the UV detection of NLAAs is of practical significance. In this study, a novel HPLC-UV method was developed for the simultaneous detection of N-lauryl glutamine (LG), N-lauryl glycine (LC), N-lauryl alanine (LA), and N-lauryl sarcosine (LS) by optimizing the mobile-phase composition and selecting an appropriate chromatographic column and detection wavelength. The samples were mixed with acetonitrile-0.10% H3PO4 aqueous solution (60∶40, v/v) and sonicated for 10 min, then stayed at room temperature for 5 min. Subsequently, the mixture was filtered through a 0.22 μm filter membrane and separated on an Agilent Eclipse Plus C18 column (150 mm×4.6 mm, 5 μm). The mobile phase used for separation consisted of acetonitrile-0.10% H3PO4 aqueous solution at a flow rate of 1.0 mL/min. The detection wavelength was set at 205 nm, and the injection volume was 10 μL. The results demonstrated that the four NLAAs exhibited good linearity in the range of 2.0-800.0 mg/L, with correlation coefficients (r)≥0.9995. The limits of detection (LODs) ranged from 0.17 to 0.49 mg/L, and limits of quantification (LOQs) ranged from 0.57 to 1.63 mg/L. The relative standard deviations (RSDs) for precision, repeatability, and stability over 24 h were all below 2.0%. Using this method, the NLAA contents of five facial-cleanser products were determined. The results demonstrated that all five samples contained one or more NLAAs, and the total NLAA contents ranged from 64.58 to 97.01 mg/g. The five spiked-sample recoveries of the NLAAs at four different spiked levels (0.60, 4.50, 15.00, 24.00 mg/g) ranged from 94.3% to 107.4%, indicating satisfactory accuracy. However, the actual NLAA composition and label for one facial-cleanser product were not consistent with our test results. This finding demonstrates the necessity of strengthening market monitoring through testing. The proposed method has the advantages of simple pretreatment, rapid testing, good precision, high accuracy, and appropriate stability. Thus, it is suitable for the determination of NLAA contents in facial cleansers and provides an effective technical reference for the raw-material purity assessment, synthetic yield detection, and product quality control of this type of surfactant.
N-月桂酰氨基酸(NLAAs)表面活性剂与传统表面活性剂相比在安全性上具有明显的优势,应用领域日益增多。但由于NLAAs的紫外吸收较弱,采用高效液相色谱-紫外检测进行含量测定存在一定困难,一般使用示差折光指数检测器、蒸发光散射检测器等通用型检测器来进行检测。为解决这一难题,本研究通过优化流动相的组成,选择合适的色谱柱和检测波长,建立了高效液相色谱-紫外检测同时测定月桂酰谷氨酸(LG)、月桂酰甘氨酸(LC)、月桂酰丙氨酸(LA)、月桂酰肌氨酸(LS)4种NLAAs表面活性剂的方法。样品在乙腈-0.10% H3PO4水溶液(60∶40, v/v)中超声提取10 min,滤膜过滤后用高效液相色谱仪测定,以乙腈-0.10% H3PO4水溶液为流动相进行梯度洗脱,经Agilent Eclipse Plus C18色谱柱(150 mm×4.6 mm, 5 μm)分离,在205 nm波长处进行检测。结果显示:4种NLAAs在2.0~800.0 mg/L范围内呈良好的线性关系,相关系数(r)均≥0.9995,检出限(LOD)为0.17~0.49 mg/L,定量限(LOQ)为0.57~1.63 mg/L。在0.60、4.50、15.00、24.00 mg/g4个加标水平下,NLAAs的加标回收率在94.3%~107.4%范围内。采用该方法对5个洗面奶样品中的NLAAs进行含量测定,发现所有样品都含有一种或多种NLAAs化合物,NLAAs的总含量在64.58~97.01 mg/g范围内。该方法前处理简单,测试快速,方法精密度、准确性、稳定性良好,适于洗面奶中NLAAs的含量测定,也可为该类型表面活性剂原料纯度、合成产率检测及产品的质量控制提供有效的技术参考。
Keywords: