XÂY DỰNG QUY TRÌNH PHÂN TÍCH ĐỒNG THỜI MỘT SỐ PHTHALAT TRONG NƯỚC SƠN MÓNG TAY BẰNG PHƯƠNG PHÁP LC-MS
Tác giả: NGUYỄN HỮU LẠC THỦY, THẠCH THỊ BÔ PHA, NGUYỄN ĐỨC TUẤN
TÓM TẮT
Summary
A highly sensitive LC-MS method was successfully developed for simultaneous analysis of 19 phthalates in nail polish product, of which six phthalates are in the prohibited list of the ASEAN Harmonization System Agreement for Cosmetic Management. The suitable chromatographic conditions were as follows: Hexyl phenyl column (100 x 2.1 mm; 1.7 µm), the column temperature at 35 oC, flow rate of 0.3 ml/min, injection volume of 5 µl, mobile phase containing mixture of methanol and acetonitrile (1:1) and 5 mM ammonium acetate solution in gradient mode. Mass analysis was performed by using an ESI source in positive mode, dry gas flow of 10 l/min, detection voltage at 5000 Volt, quadrupole temperature at 100 °C, and transfer temperature at 330 °C. The method was validated according to the guidance of USP 43 and ISO 12787:2011 for cosmetic analysis by chromatographic method. By using di-n-butyl phthalate-d4 and di-ethylhexyl phthalate-d4 as internal standard, a very good linearity range of the phthalates (0.10 – 1.00 µg/ml, R2 > 0.996) was achieved. The recoveries of the phthalates at three concentration levels (LOQ, 3LOQ, and 5LOQ) were in the range of 80.0 % – 110.0 % with the relative standard deviations of 0.1 % – 4.0 %. LOD was 0.03 µg/ml. The validated method can be applied for simultaneous determination of the phthalates in available nail polish products.
Keywords: Phthalate, nail polish, LC-MS.
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