scholarly journals Determining High-Intensity Sweeteners in White Spirits Using an Ultrahigh Performance Liquid Chromatograph with a Photo-Diode Array Detector and Charged Aerosol Detector

Molecules ◽  
2019 ◽  
Vol 25 (1) ◽  
pp. 40 ◽  
Author(s):  
Kang Ma ◽  
Xiaojia Li ◽  
Yiwen Zhang ◽  
Fei Liu

In China, white spirit is not only an alcoholic drink but also a cultural symbol. A novel and accurate method for simultaneously determining nine sweeteners (most authorized for use in China) in white spirits by ultrahigh performance liquid chromatography (UHPLC) with a photo-diode array detector (PDA) and charged aerosol detector (CAD) was developed. The sweeteners were acesulfame, alitame, aspartame, dulcin, neotame, neohesperidine dihydrochalcone, saccharin, sodium cyclamate, and sucralose. The sweeteners were separated within 16 min using a BEH C18 column and linear gradient-elution program. The optimized method allowed low concentrations (micrograms per gram) of sweeteners to be simultaneously detected. The CAD gave good linearities (correlation coefficients > 0.9936) for all analytes at concentrations of 0.5 to 50.0 μg/g. The limits of detection were 0.16 to 0.77 μg/g. Acesulfame, dulcin, neohesperidine dihydrochalcone, and saccharin were determined using the PDA detector, which gave correlation coefficients > 0.9994 and limits of detection of 0.16 to 0.22 μg/g. The recoveries were 95.1% to 104.9% and the relative standard deviations were 1.6% to 3.8%. The UHPLC-PDA-CAD method is more convenient and cheaper than LC-MS/MS methods. The method was successfully used in a major project called “Special Action against Counterfeit and Shoddy white spirits” and to monitor risks posed by white spirits in China.

Author(s):  
Sergey V. Andreev ◽  
Evgeny S. Belyaev ◽  
Anna O. Ivanova ◽  
Elvina A. Novikova ◽  
Anatoly A. Ishchenko

Chlorhexidine digluconate has been widely used in lenticular compositions, skin antiseptics and other ready-to-use disinfectants. This is due to its low toxicity, as well as a wide range of antimicrobial effects. A commonly used method for the analysis of commercially available chlorhexidine digluconate (usually available as a 20% aqueous solution) is high-performance liquid chromatography. In this article, the main methods of analysis used to determine chlorhexidine digluconate in disinfectants and skin antiseptics are considered. A new simple technique for the determination of chlorhexidine digluconate in technical products and disinfectants based on acid-base titration in alcohol-ketone is developed. It is shown that in this medium hydrochloric acid interacts with two nitrogen atoms of the chlorhexidine digluconate molecule. The end point of the titration is established by the transition of the blue color to green in the presence of bromophenol blue. The range of measured concentrations is from 0.1 to 2.0 mass%. The relative error of the method is 2.5% with the confidence probability P = 0.95. A comparison of the diode array detector and the charged aerosol detector for the determination of chlorhexidine digluconate has been performed. It is shown that a charged aerosol detector can be used to analyze chlorhexidine digluconate in cases where it is difficult to analyze with an ultraviolet or diode array detector. However, the sensitivity of the detector of charged aerosols is significantly lower than that of the diode matrix, and the linearity range is smaller. All methods were tested on model samples, as well as on samples of disinfectants, skin antiseptics, soaps and wipes with antibacterial effect.


2020 ◽  
Vol 69 (3) ◽  
pp. 151-155
Author(s):  
Yayoi KANBAYASHI ◽  
Yu TSUTSUMI ◽  
Toshimi MIZUKOSHI ◽  
Hideyuki YAMAGUCHI

2006 ◽  
Vol 89 (1) ◽  
pp. 139-143 ◽  
Author(s):  
Maria Helena Iha ◽  
Myrna Sabino

Abstract A method was developed and validated in-house for the determination of patulin (PAT), a toxic mold metabolite, in apple juice. The sample was extracted with ethyl acetatehexane and analyzed by liquid chromatography equipped with a C18 column and diode array detector. The mobile phase used for the quantification was waterethanol, at a flow rate of 0.5 mL/min. The method showed a mean recovery of 84.8%, the relative standard deviation obtained in the precision study was <7.7%, the quantification and detection limits were 7 and 3 μg/L, respectively, and the linear range for PAT in apple juice was 2.6650 μg/L. The ruggedness was evaluated by an intralaboratory experiment, in which 5 factors were studied, and only one was found to influence the observed results. The developed method is fast, practical, and simple; the solvents (except hexane) and reagents used were nontoxic. The results of the validation confirmed the efficiency of the method, which is sensitive enough to be used in studies required to quantify PAT in apple juice.


INDIAN DRUGS ◽  
2021 ◽  
Vol 57 (11) ◽  
pp. 52-62
Author(s):  
Mohanrao Tammisetty ◽  
Challa balasekhara Reddy ◽  
Puttagunta Srinivasa Babu

Specific and innovative method was developed and validated for the identification and quantification of cefixime and erdosteine in the bulk and formulation samples by UPLC with PDA detector.The analytical technique was with buffer (pH: 7.0): methanol, (65:35%, v/v) using the Sunfire C18, 5μ, 46mmX150mm analytical column with analysis time of six minutes. Flow of mobile phase through the column was 1.0 mL/min. Sample volume was 10 μL. Detection was carried at 254 nm in photo diode array detector. The retention times of cefixime and erdosteine were 2.012 min and 3.122 min., respectively. The curve indicates that correlation coefficient (r2) was superior by having the value 1.000 with linear range of 20.0 ng/mL-200.0 ng/mL for Cefixime and 30 ng/mL-300.0 ng/mL for erdosteine. The correlation coefficient (r2) for erdosteine found 1.000. The LoQ for cefixime and erdosteine was 20ng/mL and 30ng/mL respectively. The LOD for cefixime and erdosteine was 1.0 ng/mL and 1.5 ng/mL respectively. The developed method was applied for the bulk and formulation and equipement cleaning sample.


1989 ◽  
Vol 35 (3) ◽  
pp. 471-475
Author(s):  
A Jamani ◽  
M Pudek ◽  
W E Schreiber

Abstract This is a rapid (10 min per sample), highly sensitive procedure for quantifying urinary porphobilinogen (PBG). Interfering substances are removed by selectively adsorbing PBG onto an ion-exchange resin. After PBG is eluted with 0.5 mol/L formic acid, Ehrlich's reagent is added to produce the chromophore, which is then injected into a liquid chromatograph equipped with a diode-array detector. PBG is separated by a linear gradient (10% to 100%) of methanol in 10 mmol/L phosphate buffer, pH 3.0. Absorbance is monitored at 555 nm. Assay response varies linearly with PBG concentration over the range 0-110 mumol/L (0-25 mg/L). As little as 1.5 mumol/L (0.3 mg/L) can be detected. In prepared urine samples with known PBG concentrations, the within-run coefficient of variation (CV) ranged from 1.7% to 3.2%, the day-to-day CV from 3.5% to 6.1%. PBG concentrations in 24-h urine collected from 25 healthy subjects were all below the detection limit of the assay (less than 1.5 mumol/L). We used the new assay to measure PBG concentrations in the urine of two patients with latent porphyria. This method is more sensitive than spectrophotometric techniques currently used for measuring urinary PBG.


Author(s):  
Thu Dam Thi ◽  
Kieu Anh Nguyen Thi ◽  
Thanh Phuong Nguyen Thi ◽  
Hong Hanh Nguyen Thi ◽  
Dat Nguyen Thanh ◽  
...  

A method using solid phase extraction (SPE) and high performance liquid chromatography with diode array detector (HPLC-DAD) has been optimized for the simultaneous determination of notoginsenoside R1 and three ginsenosides Rg1, Re, Rb1 in solid, oil, and liquid dietary supplements. The substances were separated by an InertSustain C18 column (250 mm × 4.6 mm i.d.; particle size 5 μm) with a gradient program composed of acetonitrile and water. Linearities were in the range of 4.0 - 400 μg/mL with the coefficients of determination were more than 0.999. The limits of detection and limits of quantitation were 2.13 - 6.89 μg/g and 7.11 - 22.98 μg/g, respectively. The recovery values of the compounds were in the range of 87.2 - 103.5%. The precision study showed the intra-day relative standard deviation (RSD) of 1.41 - 2.91%, and inter-day RSD of 1.87 - 4.85%, which meet the AOAC International requirements. The method was applied to determine the content of notoginsenoside R1, ginsenoside Rg1, ginsenoside Re, and ginsenoside Rb1 in 20 dietary supplement samples containing Ginseng and Pseudoginseng.


Sign in / Sign up

Export Citation Format

Share Document