Xây dựng quy trình định lượng đồng thời 6 phathalat trong keo dán mi bằng phương pháp sắc ký khí ghép nối khối phổ GC-MS

Abstract

A highly sensitive GC-MS method was successfully developed for simultaneous analysis of 6 phthalates in eyelash adhesive products, of which four phthalates are in the prohibited list of the ASEAN Harmonization System Agreement for Cosmetic Management. The suitable chromatographic conditions were as follows: Capillary column DB – 5ms (30 m × 0.25 mm; 0.25 µm); helium as carrier gas; flow rate of 1.0 ml/min; injection volume of 1 µl in split injection mode with split ratio is 1:5; the oven temperature programmed at 50 ºC for 1 min, from 50 ºC to 280 ºC at 30 ºC min-1, held at 280 ºC for 5 min, then increased to 310 ºC at 10 ºC min-1 and held 310 ºC for 2 min; electron ionization at 70 eV; ion source temperature at 230 ºC; interface temperature at 280 °C and injection port temperature at 280 ºC; analysis mode is Scan mode. The method was validated according to the guidance of ICH topic Q2 (R1) and ISO 12787:2011 for cosmetic analysis by chromatographic method. By using di-n-butyl phthalate-d4 as internal standard, a very good linearity range of the phthalates (0.01 – 3.00 µg/ml, R2 > 0.998) was achieved. The recoveries of the phthalates at ten concentration levels (from LOQ to 300 × LOQ) were in the range of 96.40 – 106.96 % with the relative standard deviations of 0.26 – 4.60 % (n = 3). LOD was 0.003 µg/ml.