| As the strengthening of the people’s consciousness on health and surroundings, green packaging are getting more and more attention. Edible packaging as the category of the green packaging material has been widely used in foodstuff and drug. In order to increase the acceptability of foodstruff and drug, the colorants often were added for more bright-coloured and attracting attention. The industrial dyes including acid dyes and disperse dyes etc are cost-effectiveness, stability, and color-solid, some unscrupulous traders used them to color foodstruff and drug. But the dyes will be produce sensitization and carcinogenic effects and bring potential threat to the health of consumers over the long time, so the study is very necessary about the analysis of the industrial dyes in edible packaging.In this paper, the methods of qualitative and quantitative analysis has been established for detecting of 26 acid dyes, 17 allergenous disperse dyes, and 3 carcinogenic dyes in gelatin capsule and oblatum by high performance liquid chromatography with diode array detector and high performance liquid chromatography tandem mass spectrometry. The main work and conclusions are obtained as follows:(1) A high performance liquid chromatography with diode array detector(HPLC-DAD) analysis method was established for the determination of 18 acid dyes in gelatin capsule and oblatum. The different sample matrixes has different pretreatments. For gelatin capsule sample, it was extracted and purified by WAX solid phase extraction; For oblatum sample, it was extracted by acetonitrile-methanol(5:5, V/V) and purified by WAX solid phase extraction. The retention time was used and supplemented by the extracting spectra from diode array detector to obtain qualitative results. 18 acid dyes were quantified by external standard method. The analytes were separated by XDB C18 column with gradient elution using acetonitrile-20 mmol/L ammonium acetate solution(adjusting p H = 4.5 by formic acid) as the mobile phase. Under the detection wavelength of 420, 480, 520, 630 nm, the good linearity of 18 acid dyes was observed in the range of 0.25 ~ 50 μg/m L with correlation coefficient in the range of 0.9991 ~ 1.0000; The limits of detection(LODs) for 18 acid dyes were in the ranges of 0.04 ~ 0.23 μg/g, and the limits of quantitification(LOQs) were in the ranges of 0.11 ~ 0.50 μg/g. The recoveries for 18 acid dyes were 62.1 ~ 99.9%, and the relative standard deviations(RSDs) were 0.3 ~ 10.8%.(2) An analytical method of high performance liquid chromatography tandem mass spectromrtry(HPLC-MS/MS) for 22 acid dyes in gelatin capsule and oblatum was realized. A Plus C18 column was used, and the mobile phase was contained by acetonitrile-10 mmol/L ammonium acetate solution with gradient elution. The analytes were quantified by matrix matching standard curve method under the negative ion model. The good linearity of 22 acid dyes was obtained in their respective linearity ranges, and all the correlation coefficients were greater than 0.9915. LODs of 22 acid dyes were between 0.02 and 0.75 μg/g, and LOQs were between 0.03 to 2.50 μg/g. The recoveries of 22 acid dyes were in ranges of 70.5 ~ 109.5%, and RSDs were in ranges of 4.6 ~ 14.5%.(3) 17 allergenous disperse dyes and 3 carcinogenic dyes were determined in gelatin capsule and oblatum by HPLC-DAD. The sample was extracted by acetonitrile-methanol(2:2, V/V), and quantified by external standard method. The retention time and the extracting spectra from diode array detector were used to obtain qualitative results, so that avoiding “false-positive” cases happened in the process of target dyes detection. The chromatographic separation was performed on a Plus C18 column with gradient elution using acetonitrile-0.3% triethylamine solution(containing 0.2% phosphoric acid, p H = 2.7) as the mobile phase. Under the column temperature of 50 oC and the detection wavelength of 360, 420, 460, 570, and 630 nm, the good linear relationship of 20 dyes was observed within the range of 0.5 ~ 20 μg/m L with correlation coefficients ranging of 0.9991 ~ 1.0000. LODs for 20 dyes were between 0.05 and 0.27 μg/g, and LOQs were between 0.16 and 2.33 μg/g. The recoveries of 20 dyes ranged from 64.1 to 114.9% and RSDs ranged from 0.4 to 9.9%.(4) The determination of 17 allergenous disperse dyes and 3 carcinogenic dyes in gelatin capsule and oblatum by HPLC-MS/MS was developed. The sample was extracted by acetonitrile-methanol(2:2, V/V), and then analyzed in multiple reaction monitoring model. The chromatographic separation was achieved on a BEH C18 column by gradient elution. Acetonitrile-water was the mobile phase with negative ion model, and acetonitrile-5 mmol/L ammonium acetate solution(containing 0.1% formic acid) was the mobile phase with positive ion model. Sample matrix matching standard curve method was accepted. The good linearity for 20 dyes was achieved in range of 5 ~ 1000 μg/L with correlation coefficients ranging of 0.9966 ~ 1.0000. LODs and LOQs of 20 dyes were 0.01 ~ 1.60 μg/kg and 0.05 ~ 5.00 μg/kg, respectively. The recoveries of 20 dyes were 60.2 ~ 110.3% with RSDs of 1.1 ~ 10.9%. |
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