Determination of total phthalate in cosmetics using a simple three-phase sample preparation method

Abstract

A simple sample preparation method requiring minimal organic solvents is proposed for the determination of the total phthalate content in cosmetics by high-performance liquid chromatography-tandem mass spectrometry. The hydrolysis of phthalates and purification of interfering substances were performed in a three-phase system that included an upper n-hexane phase, a middle ethanol phase, and a lower aqueous alkali solution. This three-phase system utilized an incremental purification strategy. The apolar ingredients were extracted with n-hexane, the polar pigments accumulated in the ethanol phase, and the hydrolysis product, phthalic acid, remained in the hydrolysate. Under the optimized conditions, the correlation coefficients (r) for the calibration curves were 0.998-0.999 in the range 0.60-12 mol L. The limit of detection was 5.1 μmol kg, and the limit of quantification was 9.2 μmol kg. The recoveries varied from 84 to 97% with RSDs equal to or lower than 11%. The intra-day and inter-day repeatability values, expressed as the relative standard deviation, were less than 8.7 and 9.8, respectively. No obvious matrix effect existed in the different cosmetics matrices. The validated method was applied for the analysis of 57 commercial cosmetic samples. Graphical abstract Analysis of phthalates in cosmetics using a three-phase preparation method.

Phthalate sum determination in farmland soils using high‐performance liquid chromatography with tandem mass spectrometry

“…The results from a comparison of the proposed method to previously reported procedures for phthalate sum determination are shown in Table . During the hydrolysis process, this method and the other two developed by our group were much less time‐consuming than those for fatty food and urine because of the use of TBAB. Regarding clean‐up, either a large volume of organic solvent (80 mL C 2 H 5 OC 2 H 5 ) or a tedious SPE was applied; in the method for fatty food, a small volume of hexane was used because a pre‐extraction step was conducted before hydrolysis.…”

“…Chromatographic separation was carried out at 35°C on a Shim‐pack XR‐ODS column (2.2 µm, 150×3 mm) from Shimadzu. The mobile phase consisted of water (A) and methanol (B) (both containing 0.1% formic acid) and was programmed as follows: linear gradient from 15 to 95% of methanol between 0 and 7.75 min and then keeping it constant for 2 min before being returned to the initial condition in 0.25 min . The column was re‐equilibrated for 5 min at the initial mobile phase composition, obtaining a total run‐time of 15 min.…”

“…The optimized MS/MS parameters were: declustering potential −35 V, entrance potential −10 V, collision energy −15/−24 eV, and collision cell exit potential −15 V. The precursor ion was m/z 164.9 and 168.8 for the analyte and internal standard, and the product ions were 120.9 and 77 for the analyte while the product ions were 124.9 and 80.9 for the internal standard with 164.9 > 77.0 and 168.8 > 80.9 as the quantitative ions, respectively. Phthalate sum in the soil samples (containing the IS at 1.5 µg/g that was added before sample treatment) were calculated from the calibration curve obtained by plotting the ratio of analyst peak area to IS peak area against the analyte concentrations .…”

Immunological Analytical Techniques for Cosmetics Quality Control and Process Monitoring

“…A great number of immunoassays have been reported in the literature for the detection of different phthalates in food and in environmental matrices [48][49][50][51][52][53][54][55][56]. In cosmetics, the most used methods for the detection of phthalates are based on liquid chromatography [57,58]. Wei et al proposed an indirect competitive ELISA for the detection of DBP, and the technique was used to assess the presence of this target analyte in nail polish samples [59].…”

Development and validation of a dispersive liquid–liquid microextraction method for the determination of phthalate esters in perfumes using gas chromatography-mass spectrometry

“…13 Several analytical methods have been developed for the determination of PEs in cosmetic products. 9,[14][15][16][17][18][19][20][21][22][23][24][25][26][27] The most commonly used technique for the determination of PEs in perfumes is gas chromatography -mass spectrometry (GC-MS) e.g. 9,18,19,[28][29][30][31] Several studies have reported the presence PEs in perfumes in wide concentration ranges from sub ppm to high percentage.…”