scholarly journals Quantification of aniline and N-methylaniline in indigo

2021 ◽  
Vol 11 (1) ◽  
Author(s):  
Michael Cordin ◽  
Thomas Bechtold ◽  
Tung Pham

AbstractAniline and N-methylaniline are common contaminants in commercially produced indigo. It is known, that commercially produced indigo contains up to 0.6% aniline and 0.4% N-methylaniline by weight and indigo dye shows a small mutagenic effect, most probably due to the presence of these contaminants. The present work describes a new and powerful analytical method to determine the concentration of these contaminants in indigo. This method is based on the transformation of water insoluble indigo into soluble leucoindigo and allows therefore the acidic extraction of the aromatic contaminants. This transformation step is essential, because the main part of these contaminants are strongly included in the indigo crystals. The amount of extracted aniline and N-methylaniline from the leucoindigo solution was quantified with high performance liquid chromatography (HPLC, combined with a photo diode array detector). A possible accumulation of the aromatic amines at the indigo crystal surface was investigated using FTIR and by adsorption studies. Therefore this method allows an accurate monitoring of these toxic by-products in the indigo dye, which is important for an economic and environmental assessment of the denim production.

Marine Drugs ◽  
2021 ◽  
Vol 19 (6) ◽  
pp. 321
Author(s):  
Maria Orfanoudaki ◽  
Anja Hartmann ◽  
Julia Mayr ◽  
Félix L. Figueroa ◽  
Julia Vega ◽  
...  

This study presents the validation of a high-performance liquid chromatography diode array detector (HPLC-DAD) method for the determination of different mycosporine-like amino acids (MAAs) in the red alga Bostrychia scorpioides. The investigated MAAs, named bostrychines, have only been found in this specific species so far. The developed HPLC-DAD method was successfully applied for the quantification of the major MAAs in Bostrychia scorpioides extracts, collected from four different countries in Europe showing only minor differences between the investigated samples. In the past, several Bostrychia spp. have been reported to include cryptic species, and in some cases such as B. calliptera, B. simpliciuscula, and B. moritziana, the polyphyly was supported by differences in their MAA composition. The uniformity in the MAA composition of the investigated B. scorpioides samples is in agreement with the reported monophyly of this Bostrychia sp.


2013 ◽  
Vol 2013 ◽  
pp. 1-10 ◽  
Author(s):  
Thiyagarajan Sathishkumar ◽  
Ramakrishnan Baskar ◽  
Mohan Aravind ◽  
Suryanarayanan Tilak ◽  
Sri Deepthi ◽  
...  

Flavonoids are exploited as antioxidants, antimicrobial, antithrombogenic, antiviral, and antihypercholesterolemic agents. Normally, conventional extraction techniques like soxhlet or shake flask methods provide low yield of flavonoids with structural loss, and thereby, these techniques may be considered as inefficient. In this regard, an attempt was made to optimize the flavonoid extraction using orthogonal design of experiment and subsequent structural elucidation by high-performance liquid chromatography-diode array detector-electron spray ionization/mass spectrometry (HPLC-DAD-ESI/MS) techniques. The shake flask method of flavonoid extraction was observed to provide a yield of 1.2±0.13 (mg/g tissue). With the two different solvents, namely, ethanol and ethyl acetate, tried for the extraction optimization of flavonoid, ethanol (80.1 mg/g tissue) has been proved better than ethyl acetate (20.5 mg/g tissue). The optimal conditions of the extraction of flavonoid were found to be 85°C, 3 hours with a material ratio of 1 : 20, 75% ethanol, and 1 cycle of extraction. About seven different phenolics like robinin, quercetin, rutin, sinapoyl-hexoside, dicaffeic acid, and two unknown compounds were identified for the first time in the flowers of T. heyneana. The study has also concluded that L16 orthogonal design of experiment is an effective method for the extraction of flavonoid than the shake flask method.


2009 ◽  
Vol 92 (2) ◽  
pp. 680-688 ◽  
Author(s):  
Pei Chen ◽  
Renata Atkinson ◽  
Wayne R Wolf

Abstract The purpose of this study was to develop a single-laboratory validated (SLV) method using high-performance liquid chromatography with different detectors diode array detector (DAD); fluorescence detector (FLD); and mass spectrometry (MS) for determination of 7 B-complex vitamins (B1-thiamin, B2-riboflavin, B3-nicotinamide, B6-pyridoxine, B9-folic acid, pantothenic acid, and biotin) and vitamin C in multivitamin/multimineral dietary supplements. The method involves the use of a reversed-phase octadecylsilyl column (4 m, 250 2.0 mm id) and a gradient mobile phase profile. Gradient elution was performed at a flow rate of 0.25 mL/min. After a 5 min isocratic elution at 100 A (0.1 formic acid in water), a linear gradient to 50 A and 50 B (0.1 formic acid in acetonitrile) at 15 min was employed. Detection was performed with a DAD as well as either an FLD or a triple-quadrupole MS detector in the multiple reaction monitoring mode. SLV was performed using Standard Reference Material (SRM) 3280 Multivitamin/Multimineral Tablets, being developed by the National Institute of Standards and Technology, with support by the Office of Dietary Supplements of the National Institutes of Health. Phosphate buffer (10 mM, pH 2.0) extracts of the NIST SRM 3280 were analyzed by the liquid chromatographic (LC)-DAD-FLD/MS method. Following extraction, the method does not require any sample cleanup/preconcentration steps except centrifugation and filtration.


Molecules ◽  
2020 ◽  
Vol 25 (19) ◽  
pp. 4581 ◽  
Author(s):  
Eui-Jeong Doh ◽  
Guemsan Lee ◽  
Hyun-Jong Jung ◽  
Kang-Beom Kwon ◽  
Jung-Hoon Kim

Amomi Fructus is widely used to treat digestive disorders, and Amomum villosum, A. villosum var. xanthioides, and A. longiligulare are permitted medicinally in national pharmacopeias. However, there are a variety of adulterants present in herbal markets owing to their morphological similarities to the genuine Amomum species. Forty-two Amomi Fructus samples from various origins were identified using internal transcribed spacer and chloroplast barcoding analyses, and then their chromatographic profiles were compared using chemometric analysis for chemotaxonomic monitoring. Among the Amomi Fructus samples, A. villosum, A. longiligulare, A. ghaticum, and A. microcarpum were confirmed as single Amomum species, whereas a mixture of either these Amomum species or with another Amomum species was observed in 15 samples. Chemotaxonomic monitoring results demonstrated that two medicinal Amomum samples, A. villosum and A. longiligulare, were not clearly distinguished from each other, but were apparently separated from other non-medicinal Amomum adulterants. A. ghaticum and A. microcarpum samples were also chemically different from other samples and formed their own species groups. Amomum species mixtures showed diverse variations of chemical correlations according to constituent Amomum species. Genetic authentication-based chemotaxonomic monitoring methods are helpful in classifying Amomi Fructus samples by their original species and to distinguish genuine Amomum species from the adulterants.


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