scholarly journals Application of targeted 2D planar chromatography in the control of ginkgolic acids in some herbal drugs and dietary supplements

2020 ◽  
Vol 70 (2) ◽  
pp. 201-213
Author(s):  
Piotr Migas ◽  
Anna Romańczuk ◽  
Marta Szumacher ◽  
Mirosława Krauze-Baranowska
Keyword(s):  
Formic Acid ◽  
Dietary Supplements ◽  
Extraction Method ◽  
Chromatographic Method ◽  
Herbal Drugs ◽  
Sample Matrix ◽  
Mobile Phases ◽  
First Time ◽  
Ginkgolic Acids

AbstractTwo-step targeted 2D planar chromatographic method (2DTLC) was used in the determination of ginkgolic acids in pharmaceuticals and dietary supplements. The choice of the extraction method and the separation technique was guided by the formulation type (capsule, tablet, tincture) with expected low amounts of ginkgolic acids in the analyzed herbal samples. Separation of ginkgolic acids C15:1 and C17:1 on HPTLC RP18 WF254s was preceded by its separation from the sample matrix on TLC Si60 F254s. Mobile phases consisted of acetonitrile/water/formic acid (80:20:1, V/V/V) and n-heptane/ethyl acetate/formic acid (20:30:1, V/V/V), resp. Identification of separated compounds was based on 2D-TLC co-chromatography with reference substances and off-line 2D-TLC x HPLC-DAD-ESI-MS analysis. Quantification of ginkgolic acids C15:1 and C17:1 was conducted densitometrically. Among the analyzed products, the presence of ginkgolic acids was confirmed only in herbal drugs containing 60 % ethanolic tinctures of Ginkgo biloba leaves. The use of TLC in the quantification of ginkgolic acids C15:1 and C17:1 in ginkgo extracts was described for the first time.

scholarly journals Simultaneous Determination of Five Chromones of Radix Saposhnikoviae Extract in Rat Plasma by UPLC-MS/MS: Application to a Comparative Pharmacokinetic Study in Normal and Febrile Rats

2019 ◽  
Vol 2019 ◽  
pp. 1-11
Author(s):  
Li Meng ◽  
Hui Gao ◽  
Bin Chen ◽  
Peng-peng Liu ◽  
Guo-shun Shan ◽  
...  
Keyword(s):  
Formic Acid ◽  
Simultaneous Determination ◽  
Ultra Performance Liquid Chromatography ◽  
Rat Plasma ◽  
Active Components ◽  
Mobile Phases ◽  
The Matrix ◽  
Acquity Uplc ◽  
First Time

A rapid and sensitive quantitative analytical method was established for the simultaneous determination of five chromones (prim-O-glucosylcimifugin, cimifugin, 4′-O-β-D-glucosyl-5-O-methylvisamminol, 5-O-methylvisammiol, and sec-o-glucosylhamaudol) in the plasma of RS-treated rats for the first time using ultra performance liquid chromatography- (UPLC-) tandem mass spectrometry. The Waters Acquity UPLC BEH C18 (50 mm × 2.1 mm, 1.7 μm) was used as the chromatographic column, 0.1% formic acid water and 0.1% formic acid acetonitrile comprised the mobile phases, and all samples were determined under positive ion mode. The results showed that all analytes had good linearity (r>0.9902), between-day and within-day precisions less than 15%, accuracy between −5.50% and 5.53%, and extraction recovery between 88.26% and 97.65%. Both the matrix effect and stability met the requirements. This method was successfully applied for the comparative pharmacokinetics of five active components of RS in normal and febrile rats. The results showed that the pharmacokinetic behavior of RS extract significantly differed between the two types of rats.

A Headspace Gas Chromatographic Method for Determination of Formic acid Content in Isosulfan Blue and in Various Drugs

2021 ◽  
Vol 37 (2) ◽  
pp. 321-329
Author(s):  
Nilesh Takale ◽  
Neelakandan Kaliyaperumal ◽  
Gopalakrishnan Mannathusamy ◽  
Rajarajan Govindasamy
Keyword(s):  
Sulfuric Acid ◽  
Formic Acid ◽  
Chromatographic Method ◽  
Isopropyl Alcohol ◽  
Class Iii ◽  
Drug Substances ◽  
Headspace Gas ◽  
Concentrated Sulfuric Acid ◽  
Gas Chromatographic Method

The Pharmaceutical industry uses formic acid in the manufacturing of various drug substances or API. At the time of manufacturing of API formic acid is use as an oxidizing agent. Formic acid is the simplest carboxylic acid. It also called methanoic acid.Formic acid present in API at high concentrations is very hazardous but in low concentrations is very beneficial. The developed and validated method was short, precise, cost effective and reproducible with FID detector and easy to use. The method is a selective and superficial analytical method for determination of formic acid in different drug substances. We report here the development and validation study of headspace gas chromatographic method to determine formic acid in different drug substances we are reported here. As per this method, the drug sample was dissolved in 0.1% (v/v) of concentrated sulfuric acid in isopropyl alcohol (IPA) in a GC headspace vial and 0.1% (v/v) of concentrated sulfuric acid in isopropyl alcohol used as a diluent. A AB-Inowax capillary column (30 m x 0.32 mm I.D. and 0.5 µm film thickness) was used under gradient conditions with FID. The formic acid peak was well separated from all other solvents that are used in synthesis of particular drug substance. The LOD and LOQof the method for formic acid are 82 ppm and 249 ppm respectively. Formic acid are low toxic class-III solvent as per ICH guideline.

scholarly journals Single-Laboratory Validation of a High-Performance Liquid Chromatographic-Diode Array Detector-Fluorescence Detector/Mass Spectrometric Method for Simultaneous Determination of Water-Soluble Vitamins in Multivitamin Dietary Tablets

2009 ◽  
Vol 92 (2) ◽  
pp. 680-688 ◽  
Author(s):  
Pei Chen ◽  
Renata Atkinson ◽  
Wayne R Wolf
Keyword(s):  
Formic Acid ◽  
Dietary Supplements ◽  
High Performance ◽  
Array Detector ◽  
Diode Array ◽  
Diode Array Detector ◽  
Fluorescence Detector ◽  
Liquid Chromatographic ◽  
Single Laboratory

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.

scholarly journals Simultaneous Determination of 12 Marker Components in Yeonkyopaedok-san Using HPLC–PDA and LC–MS/MS

2020 ◽  
Vol 10 (5) ◽  
pp. 1713 ◽  
Author(s):  
Chang-Seob Seo ◽  
Hyeun-Kyoo Shin
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Formic Acid ◽  
Coefficient Of Determination ◽  
Photodiode Array Detection ◽  
Mobile Phases ◽  
Photodiode Array ◽  
Array Detection ◽  
Aqueous Formic Acid

Yeonkyopaedok-san is a traditional Korean medicine used in the early treatment of boils. In the present study, its 12 marker components for quality control were determined using high-performance liquid chromatography (HPLC) with photodiode array detection and ultra-performance liquid chromatography–mass spectrometry with tandem mass spectrometry (UPLC–MS/MS). The investigated 12 marker components of Yeonkyopaedok-san were as follows: 3-caffeoylquinic acid, cimifugin 7-glucoside, liquiritin apioside, ferulic acid, narirutin, 5-O-methylvisammioside, naringin, neohesperidin, oxypeucedanin hydrate, arctigenin, glycyrrhizic acid, and 6-gingerol. The analytical column used for the separation of the 12 marker analytes in Yeonkyopaedok-san was a Waters SunFire C18 column (4.6 mm × 250 mm, 5 μm). The two mobile phases used were 0.1% (v/v) aqueous formic acid and 0.1% (v/v) formic acid in acetonitrile. In the UPLC–MS/MS analysis, all components were separated using a Waters ACQUITY UPLC BEH C18 column (2.1 mm × 100 mm, 1.7 μm). The two mobile phases used were 0.1% (v/v) aqueous formic acid and acetonitrile. The coefficient of determination of the calibration curves in both analysis systems showed good linearity (>0.99). The amounts of the 12 marker components in Yeonkyopaedok-san determined using HPLC–photodiode array detection and UPLC–MS/MS analyses were found to be 0.14–9.00 mg/g and 2.35–853.11 μg/g, respectively.

Determination of creatine kinase MB activity with the Du Pont aca: interferences from the sample matrix.

1984 ◽  
Vol 30 (2) ◽  
pp. 238-242 ◽  
Author(s):  
W Stein ◽  
J Bohner
Keyword(s):  
Creatine Kinase ◽  
Protein Concentration ◽  
Chromatographic Method ◽  
Chloride Concentration ◽  
Sample Matrix ◽  
Creatine Kinase Mb ◽  
The Matrix ◽  
Enzyme Pattern ◽  
Creatine Kinase Isoenzyme Mb

Abstract During the last three years we and other have observed discrepancies between results for creatine kinase isoenzyme MB as measured with the mechanized ion-exchange chromatographic method in the Du Pont aca and those by other techniques. These observations prompted us to investigate the influence of the matrix on the Du Pont CK-MB assay. We conclude that, apart from possible interferences by CK-MM, CK-BB, and both types of macro CK, the aca will give apparent CK-MB activities that are directly related to protein concentration and inversely related to sodium chloride concentration. Practical consequences for the routine and emergency laboratories are: no diluted samples are allowed; application is restricted to samples from patients suspected of acute myocardial infarction which show upper-normal total CK activity; and multiple timed samples are run, in order to recognize the typical change in enzyme pattern with time.

Cheap pencil graphite electrodes for rapid voltammetric determination of chlorogenic acid in dietary supplements

2016 ◽  
Vol 8 (35) ◽  
pp. 6537-6544 ◽  
Author(s):  
I. G. David ◽  
D. E. Popa ◽  
M. Buleandra ◽  
Z. Moldovan ◽  
E. E. Iorgulescu ◽  
...  
Keyword(s):  
Chlorogenic Acid ◽  
Dietary Supplements ◽  
Graphite Electrode ◽  
Voltammetric Determination ◽  
Pencil Graphite Electrode ◽  
Green Coffee ◽  
Graphite Electrodes ◽  
First Time

A disposable pencil graphite electrode was used for the first time for rapid voltammetric determination of chlorogenic acid in green coffee dietary supplements.

scholarly journals A Headspace Gas Chromatographic Method for Determination of Formic Acid Content in Isosulfan Blue and Various Drug Substances

2021 ◽  
Vol 37 (02) ◽  
pp. 321-329
Author(s):  
Nilesh Takale ◽  
Neelakandan Kaliyaperumal ◽  
Gopalakrishnan Mannathusamy ◽  
Rajarajan Govindasamy
Keyword(s):  
Sulfuric Acid ◽  
Formic Acid ◽  
Chromatographic Method ◽  
Isopropyl Alcohol ◽  
Class Iii ◽  
Drug Substances ◽  
Headspace Gas ◽  
Concentrated Sulfuric Acid ◽  
Gas Chromatographic Method

The Pharmaceutical industry uses formic acid in the manufacturing of various drug substances or API. At the time of manufacturing of API formic acid is use as an oxidizing agent. Formic acid is the simplest carboxylic acid. It also called methanoic acid.Formic acid present in API at high concentrations is very hazardous but in low concentrations is very beneficial. The developed and validated method was short, precise, cost effective and reproducible with FID detector and easy to use. The method is a selective and superficial analytical method for determination of formic acid in different drug substances. We report here the development and validation study of headspace gas chromatographic method to determine formic acid in different drug substances we are reported here. As per this method, the drug sample was dissolved in 0.1% (v/v) of concentrated sulfuric acid in isopropyl alcohol (IPA) in a GC headspace vial and 0.1% (v/v) of concentrated sulfuric acid in isopropyl alcohol used as a diluent. A AB-Inowax capillary column (30 m x 0.32 mm I.D. and 0.5 µm film thickness) was used under gradient conditions with FID. The formic acid peak was well separated from all other solvents that are used in synthesis of particular drug substance. The LOD and LOQof the method for formic acid are 82 ppm and 249 ppm respectively. Formic acid are low toxic class-III solvent as per ICH guideline.

Single-Laboratory Validation of a Method for the Determination of Vitamin D3 in Dietary Supplements by Liquid Chromatography with Tandem Mass Spectrometry (LC-MS/MS)

2014 ◽  
Vol 97 (2) ◽  
pp. 403-408
Author(s):  
Victor K M Lam ◽  
Ray C T Hung ◽  
Ella L M Wong ◽  
Johnny Y W Fok ◽  
Yiu-Chung Wong
Keyword(s):  
Formic Acid ◽  
Dietary Supplements ◽  
Vitamin D3 ◽  
Time Window ◽  
Collaborative Study ◽  
Internal Standard ◽  
Ammonium Formate ◽  
Soft Gels ◽  
Single Laboratory

Abstract A single-laboratory validation (SLV) for the analysis of vitamin D3 was performed in four types of dietary supplements (capsules, soft gels, syrups, and tablets) using LC-MS/MS. Samples were treated by alkaline saponification for oil-based soft gels and utilized EDTA solution for capsules, syrups,and tablets prior to n-hexane extraction. Vitamin D3 in sample extracts was separated on a reversed-phase C18 column (100 × 2.1 mm, 2.7 μm) using a mobile phase of a 95 + 5 (v/v) mixture of 5 mM ammonium formate in methanol containing 0.1% formic acid and 5 mM ammonium formate in 0.1% formic acid running at a flow rate of 0.2 mL/min. Vitamin D3 was confirmed by the presence of three fragment ions at m/z 107, 159, and 259 within a defined retention time window from the precursor ion at m/z 385. Quantitation was based on the peak area at m/z 367 to that of the internal standard (d3-vitamin D3) at m/z 370 with reference to the respective response ratios of the calibration standards. The linear response of vitamin D3 ranged from 0.10 to 6.29 mg/L and the correlation coefficient (r) of the six-point calibrationcurves was >0.999. Accuracy, in terms of the spiked recoveries from blank syrup and starch powder at three different concentration levels, was 101–103%. Precision, determined by two different analysts over a period of 5 weeks, ranged from 2.7 to 7.0%for the four preparations. The SLV demonstrates the present LC-MS/MS method is reliable and robust for the determination of vitamin D3 in the studied dietary supplements. Considering the attainmentof satisfactory SLV results, further validation through intra-laboratory collaborative study is recommended.

scholarly journals YOUDEN'S TEST FOR CHROMATOGRAPHIC DETERMINATION OF ENALAPRIL IN PHARMACEUTICALS

2020 ◽  
Vol 5 (2) ◽  
pp. 83-87
Author(s):  
L. S. Logoyda
Keyword(s):  
Chromatographic Method ◽  
Holistic Approach ◽  
Chromatographic Determination ◽  
Hplc Method ◽  
Hplc Assay ◽  
Particle Technology ◽  
Interlaboratory Studies ◽  
Validation Procedure ◽  
First Time

Background. Robustness tests were firstly introduced for avoiding problems in interlaboratory studies and identifying the factors potentially responsible. A robustness test performing in late validation procedure involves the possibility that when the method is established not robust, it should be redeveloped and optimized. At this stage much effort has been made and money spent for optimization and validation, and therefore avoiding this would be great. Objective. The aim of the study was to consider the robustness of HPLC determination of enalapril (in tablets) by the Youden’s test. Methods. Youden’s test was chosen as an efficient method to assess the robustness among all analytical methods that is by means of an experiment design, which involved seven analytical parameters combined in eight tests. In previous studies, we evaluated the chromatographic method robustness to quantify enalapril (in tablets) by Youden’s test. Results. According to the Youden’s test criteria, HPLC method proved to be greatly robust regarding the enalapril content in introduction of variation of seven analytic parameters. The lowest variation in enalapril content was 0.91 %, when Grace Platinumр C8 EPS column (4.6 mm i.d. X 250 mm, 5 μm) was used. A holistic approach concerning simultaneous innovations in particle technology and instrument design was endeavored for the first time to meet and tackle the analytical laboratory issues. This was aimed at promoting success of analytical scientists as well as profitability and productiveness of business.  Conclusion. The Youden’s test has been proved to be an efficient and useful tool for evaluation of robustness of enalapril HPLC assay.

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