Zhong Zhixiong, Li Gongke, Zhu Binghui, Luo Zhibin, Wu Ximei
Center for Disease Control and Prevention of Guangdong Province, Guangzhou 510300, China.
Se Pu. 2010 Jul;28(7):702-7. doi: 10.3724/sp.j.1123.2010.00702.
A method for the simultaneous determination of ammonium and six alkylamines in cosmetic products by ion chromatography (IC) was developed. The sample pretreatment process and the separation resolution of chromatography were investigated. The samples were extracted by 100 mmol/L acetic acid-20% (v/v) acetonitrile solution at room temperature, and then solid phase extraction (SPE) column was used to eliminate the interferences. The influences of pH value, organic solvent and coexisted ions were investigated. The separation was carried out on IonPac CS17 (250 mm x 4 mm)analytical column and IonPac CG17 (50 mm x 4 mm)guard column using 1.5 - 15 mmol/L methanesulfonic acid and 0.5% - 5% (v/v) acetonitrile gradient elution at a flow rate of 1.0 mL/min at 24 degrees C, coupled with suppressed conductivity detector. Under the optimum conditions, a measurement could be completed less than 26 min. The linearity ranged from 0.3 to 15 mg/L, the detection limits and the quantification limits were in the ranges of 2.1 - 7.9 mg/kg and 7 - 26 mg/kg, respectively. The method was successfully employed for the determination of ammonium, methylamine, dimethylamine, trimethylamine, ethylamine, propylamine and butylamine in samples including cleaning, body lotion, skin-bleaching, sun block, marcel, hair dye and pilatory cosmetics with the recoveries of 80.2% - 109.2% and the relative standard deviations (RSDs) of 0.5% - 3.1%. The method offered high selectivity, sensitivity, and gave satisfactory results for real sample analysis.
建立了一种采用离子色谱法（IC）同时测定化妆品中铵和六种烷基胺的方法。研究了样品预处理过程和色谱分离效果。样品在室温下用100 mmol/L乙酸-20%（v/v）乙腈溶液萃取，然后使用固相萃取（SPE）柱消除干扰。考察了pH值、有机溶剂和共存离子的影响。分离在IonPac CS17（250 mm×4 mm）分析柱和IonPac CG17（50 mm×4 mm）保护柱上进行，使用1.5 - 15 mmol/L甲磺酸和0.5% - 5%（v/v）乙腈梯度洗脱，流速为1.0 mL/min，柱温24℃，配备抑制型电导检测器。在最佳条件下，不到26分钟即可完成一次测定。线性范围为0.3至15 mg/L，检测限和定量限分别在2.1 - 7.9 mg/kg和7 - 26 mg/kg范围内。该方法成功用于测定清洁、身体乳液、美白、防晒、烫发、染发和脱毛化妆品等样品中的铵、甲胺、二甲胺、三甲胺、乙胺、丙胺和丁胺，回收率为80.2% - 109.2%，相对标准偏差（RSD）为0.5% - 3.1%。该方法具有高选择性、高灵敏度，对实际样品分析结果令人满意。
