Indigotin, indirubin, berberine, palmatine, alizarin, and purpurin are major pigments of indigo plant, Phellodendron bark, and madder. The six pigments were examined using the HPLC-DAD-MS instrument for the purpose of the simultaneous detection of the pigments in a single sample run. The HPLC-DAD-MS...
Indigotin, indirubin, berberine, palmatine, alizarin, and purpurin are major pigments of indigo plant, Phellodendron bark, and madder. The six pigments were examined using the HPLC-DAD-MS instrument for the purpose of the simultaneous detection of the pigments in a single sample run. The HPLC-DAD-MS method examined the individual pigment solutions in DMSO, a solution containing 6 pigments, and the DMSO extract of the silk dyed with a dye solution of 5 pigments excluding indirubin. The retention times of the HPLC chromatograms, ${\lambda}_{max}$ of the uv-vis absorption bands in the DAD analyses, and the molecular ions detected for the compound peaks in the MSD analyses were consistent throughout the analyses of individual pigment solutions, mixed pigment solutions, and dye extracted from silk dyeing. The developed instrumental method of the simultaneous detection of six pigments can identify dye in an exhumed textile if the textile is dyed using any one (or multiple) pigments of indigo, Phellodendron bark, or madder plant.
Indigotin, indirubin, berberine, palmatine, alizarin, and purpurin are major pigments of indigo plant, Phellodendron bark, and madder. The six pigments were examined using the HPLC-DAD-MS instrument for the purpose of the simultaneous detection of the pigments in a single sample run. The HPLC-DAD-MS method examined the individual pigment solutions in DMSO, a solution containing 6 pigments, and the DMSO extract of the silk dyed with a dye solution of 5 pigments excluding indirubin. The retention times of the HPLC chromatograms, ${\lambda}_{max}$ of the uv-vis absorption bands in the DAD analyses, and the molecular ions detected for the compound peaks in the MSD analyses were consistent throughout the analyses of individual pigment solutions, mixed pigment solutions, and dye extracted from silk dyeing. The developed instrumental method of the simultaneous detection of six pigments can identify dye in an exhumed textile if the textile is dyed using any one (or multiple) pigments of indigo, Phellodendron bark, or madder plant.
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제안 방법
An Agilent 1200 series binary HPLC-DAD-MS system (Foster City, CA) equipped with a diode-array detector (DAD) and a mass selective detector (MSD) consisting of a single quadrupole mass analyzer was used for sample analysis. The mass detector was operated in both Selective Ion Monitoring (SIM) mode and Scan Mode using the atmospheric pressure chemical ionization (APCI) source in the positive ionization mode.
In this paper, the HPLC-DAD-MS instrument was used to examine the six major pigments which belong to indigo plant, Phellodendron bark, and madder plant for the purpose of detecting the six pigments simulta- neously in a single sample run. First, six dye solutions of individual pigment were examined, and second a dye solution containing all six pigments was examined using the HPLC-DAD-MS method to detect the six pigment compounds from the samples. The investigation of mixed dye solution was intended to simulate the possibility of composite dyeing of two or more dyes in one fabric, which was often practiced in the past to produce a mid-hue.
In this paper, the HPLC-DAD-MS instrument was used to examine the six major pigments of indigo plant, Phellodendron bark, and madder in DMSO sol- vent for the purpose of detecting the six pigments simultaneously in a single sample run. When the individual pigment solutions were examined, indigotin, indirubin, berberine, palmatine, alizarin, and purpurin eluted at 9.
In this paper, the HPLC-DAD-MS instrument was used to examine the six major pigments which belong to indigo plant, Phellodendron bark, and madder plant for the purpose of detecting the six pigments simulta- neously in a single sample run. First, six dye solutions of individual pigment were examined, and second a dye solution containing all six pigments was examined using the HPLC-DAD-MS method to detect the six pigment compounds from the samples.
The DMSO extract was filtered using the glass fiber enhanced 0.45µm syringe filters into an HPLC vial and the sample was analyzed using the HPLC-DAD-MS instrument.
The above results of the mixed pigment solution indicated that the six pigments can be simultaneously detected by a single sample run using the HPLC-DADMS method developed in this study. The result also implies that each pigment compound can be detected even when the exhumed textiles were dyed using any two or multiple of indigo, Phellodendron bark, and madder plant, and also when the staining of dye from adjacent clothing artifact occurred within the coffin burial.
The chemical characteristics of the six pigments are shown in [Table 1]. The method developed in this research can be applied in the future identification of dye in the exhumed textiles which have been dyed with indigo, Phellodendron bark, and madder.
The HPLC-DAD-MS results of mixed pigment solution and the extraction from the silk dyeing were consistent with those of the individual pigment solutions. The results of this study indicated that the six pigments can be simultaneously detected by a single sample run using the HPLC-DAD-MS method developed in this study. The developed instrumental method of simultaneous detection of six pigments can be used to identify dye in exhumed textiles if the textile has been dyed in the past using any one or multiple of indigo, Phellodendron bark, and madder plant.
대상 데이터
Dimethyl sulfoxide (DMSO, HPLC grade), acetonitrile (HPLC grade), HPLC water (HPLC grade), and sodium hydrosulfite were purchased from Fisher Scientific (Fair Lawn, New Jersey, USA). Formic acid (88%, ACS grade) was purchased from Macron Chemicals (Phillipsburg, NJ, USA). Aluminium potassium sulfate was purchased from Shinyo Pure Chemicals (Osaka, Japan).
Indigotin (95%), indirubin, alizarin, berberine chloride form (berberine in the following) (97%), palmatine chloride hydrate (palmatine in the following) were purchased from Sigma-Aldrich (St. Louis, MO, USA). Purpurin (85%) was purchased from Tokyo Chemical Industry (Tokyo, Japan).
Indigo, Phellodendron bark and madder were selected based on the fact that they were the most representative dyestuffs of the past which color the fabrics in blue, yellow, and red color types, and also because their major pigments with high purity can be purchased from the reliable global vendors. The six pigments under investigation were indigotin and indirubin of indigo plant, berberine and palmatine of Phellodendron bark, and alizarin and purpurin of madder. The chemical characteristics of the six pigments are shown in [Table 1].
성능/효과
The mass spectrum of each pigment peak gave the same molecular ion [M+H]+ or [M+H2]+ as those of the individual pigment solutions. The results indicate that the HPLC-DAD-MS method developed in this study, toge-ther with the present method of extracting the dye from fiber, can be used to detect and identify indigotin (and highly likely indirubin as well), berberine, palmatine, alizarin, and purpurin from the textile sample.
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