QuEChERS-同位素内标-高效液相色谱-串联质谱法同时测定化妆品中的维生素D和K

Simultaneous Determination of Vitamins D and K in Cosmetics by QuEChERS-High Performance Liquid Chromatography-tandem Mass Spectrometry with Isotope Internal Standard Method

关键词:  QuEChERS  同位素内标  高效液相色谱-串联质谱法  维生素D  维生素K

Key words:  QuEChERS  isotope internal standard  HPLC-MS/MS  vitamin D  vitamin K

摘要:

目的 采用QuEChERS-同位素内标-高效液相色谱-串联质谱法建立同时测定5种不同基质类型(液态水基类、乳液类、膏霜类、凝胶类、粉类)化妆品中维生素D和K的分析方法。方法 样品经乙腈超声提取并通过优化的QuEChERS (150 mg硫酸镁、50 mg PSA)获得净化液，采用ACQUITY UPLC BEH C18 (2.1×50 mm，1.7 μm)色谱柱，以甲醇(含0.05%甲酸，v/v；5mmol甲酸铵)为流动相，电喷雾正离子模式(ESI+)，多反应离子检测(MRM)扫描方式进行检测，以同位素内标法准确定量。结果 维生素D (D2、D3)和K (K1、K2)在5～500 ng?mL-1范围内线性关系良好，线性相关系数r均大于0.995，检出限和定量限分别为0.01 μg?g-1和0.03 μg?g-1，在3个加标水平下，液态水基类、乳液类、膏霜类、凝胶类、粉类的回收率分别为94.0%~110.1%、89.4%~111.5%、90.1%~106.8%、93.8%~109.7%和89.9%~106.2%，相对标准偏差均小于8.0%。结论 该方法操作简便、灵敏度高、结果准确，适用于化妆品中维生素D和K的测定。

Abstract:

OBJECTIVE To establish a QuEChERS-high performance liquid chromatography-tandem mass spectrometry with isotope internal standards method for the simultaneous determination of vitamins D and K in 5 different matrixes of cosmetics (water aqua, lotion, cream, gel and powder). METHODS Samples were ultrasonically extracted by acetonitrile, and then purified by optimized QuEChERS method (150 mg magnesium sulfate, 50 mg PSA). The separation was performed on an ACQUITY UPLC BEH C18 (2.1×50 mm, 1.7 μm) column using methanol (containing 0.05% formic acid, v/v; 5mmol ammonium formate) as the mobile phase. The determination was performed by MS/MS in electrospray ionization positive mode (ESI+) and multiple reaction monitoring (MRM) mode, and isotope internal standard method was used for quantitative analysis. RESULTS The linear relationship of vitamins D (D2, D3) and K (K1, K2) was good in the concentration range of 5-500 ng?mL-1, and the correlation coefficients (r) were all larger than 0.995. The limits of detection and limits of quantification were 0.01 μg?g-1 and 0.03 μg?g-1, respectively. At 3 different concentrations, the recoveries of water aqua, lotion, cream, gel and powder samples were 94.0%-110.1%, 89.4%-111.5%, 90.1%-106.8%, 93.8%-109.7% and 89.9%-106.2%, respectively. The RSD were all less than 8.0%. CONCLUSION This method is simple, sensitive and accurate, which is suitable for the determination of the vitamins D and K in cosmetics.