scholarly journals Determinations of Labile Nutrients (Methylcobalamin, 5-Methyltetrahydrofolate, and Trans Menaquinone-7) in Oil- and Beadlet-Filled, Gastric-Resistant Capsule

2020 ◽  
Vol 4 (Supplement_2) ◽  
pp. 1183-1183
Author(s):  
Hong You ◽  
Yuhao Yin ◽  
Kangzi Ren ◽  
Zhiyan Liu ◽  
Jeffrey Whaley ◽  
...  
Keyword(s):  
Dietary Supplements ◽  
Analytical Methods ◽  
The United States ◽  
Nutrient Delivery ◽  
Funding Sources ◽  
Rp Hplc ◽  
Accuracy And Precision ◽  
Relative Standard ◽  
On Line ◽  
Superficially Porous Particles

Abstract Objectives The dietary supplement industry has grown substantially, and advances in technology have played important roles in the development of new forms of dietary supplements and delivery systems. While it is recommended to use compendia methods for testing dietary supplements, the analytical methods in place are often developed for single ingredients or simple matrices and are not always fit to be used for solving modern matrix challenges. Oil- and beadlet-filled, gastric acid-resistant capsule (OBGRC) is designed to improve nutrient delivery and absorption. However, it is challenging to accurately analyze labile nutrients in OBGRCs because nutrients within different physical locations are difficult to separate, and lengthy sample preparations lead to nutrient degradation. We developed and validated analytical methods to determine methylcobalamin (MeB12), 5-methyltetrahydrofolate (5-MTHF), and trans menaquinone-7 (MK-7) in OBGRCs. Methods MeB12 and 5-MTHF were extracted by completely dissolving the OBGRC shells using aqueous buffers and then applying hexane-facilitated liquid-liquid extraction to remove the oil phase and determined by RP-HPLC using superficially porous particles columns. For MK-7 analysis, the whole OBGRC was cut to open and the oil phase was collected to dissolve in a mixture of dimethyl sulfoxide/tetrahydrofuran/ethanol before analyzed by RP-HPLC with fluorescence detection after on-line, post-column zinc reduction. The methods were subjected to single-laboratory validations according to the United States Pharmacopeia (USP) guidelines for linearity, suitability, detection limits, specificity, accuracy, and precision. Results The methods achieved chromatographic resolution of target analytes without the expensive requirement of ultra-high pressure liquid chromatography and/or mass spectrometry. The methods have wide analytical ranges (from at least 50% to 250% of the input concentrations), high precision (repeatability relative standard deviations ranging from 1.04% to 4.90%), and high accuracy (spike recovery rate ranging from 89.2% to 108%). Conclusions All three methods passed USP method validation criteria and have the potential to be widely adopted to analyze MeB12, 5-MTHF, and MK-7 in similar matrices for quality control purposes. Funding Sources The research funding was provided by Ritual and Eurofins.

scholarly journals Simultaneous Determination of Piracetam and Citicoline in Combination Drug Products by Rp-Hplc Method

2021 ◽  
pp. 171-185
Author(s):  
Meka. Srinivasa Rao ◽  
K. Rambabu
Keyword(s):  
Hplc Method ◽  
Simultaneous Estimation ◽  
Combination Drug ◽  
Drug Products ◽  
Rp Hplc ◽  
Accuracy And Precision ◽  
Ich Guidelines ◽  
System Suitability ◽  
Relative Standard

In this paper a simple, accurate and precise RP-HPLC method for the simultaneous. Estimation of piracetam and citicoline in synthetic mixtures has been developed and validated. Separation of drugs was carried out using buffer and Acetonitryle with proportion of 60:40 %v/v as mobile phase at 5 min. run time and 265nm. The Rt value for piracetam and citicoline was found to be 3.158 and 5.196 min respectively. The developed method has been validated for linearity, accuracy and precision, LOD, LOQ, and system suitability according to ICH guidelines. The low values of LOD and LOQ illustrate that the developed method was sensitive, accurate, and precise as it can detected and quantify with very low concentration. The low % RSD values below 2 indicate that the method is precise. The above validation studies revealed the method is specific, rapid, reliable, and reproducible. The high recovery and low relative standard deviation confirm the suitability of the method for routine determination of piracetam and citicoline in combined dose products.

scholarly journals Determination of Active Vitamin B12 (Cobalamin) in Dietary Supplements and Ingredients by Reversed-phase Liquid Chromatography (P13-040-19)

2019 ◽  
Vol 3 (Supplement_1) ◽  
Author(s):  
Hong You
Keyword(s):  
Liquid Chromatography ◽  
Vitamin B12 ◽  
High Performance ◽  
Reversed Phase ◽  
Hplc Method ◽  
Funding Sources ◽  
Accuracy And Precision ◽  
Relative Standard ◽  
Analysis Center ◽  
Micronutrient Malnutrition

Abstract Objectives Vitamin B12 dietary supplement can be critical to the alleviation strategies against micronutrient malnutrition and food insecurity. A high-performance liquid chromatography with ultraviolet detection (HPLC-UV) method has been developed and validated, for the quantitation of four bioactive forms of vitamin B12 (adenosylcobalamin, cyanocobalamin, hydroxocobalamin, methylcobalamin) from dietary ingredients and supplements. Methods A Plackett-Burman factorial study was used to identify factors that contributed to the extraction of cobalamins. Significant factors were selected to produce the improved HPLC method for cobalamin separation. This method was then subjected to a single-laboratory validation according to the AOAC International guidelines for linearity, suitability, detection limits, accuracy, and precision. Results The method achieves chromatographic baseline resolution of vitamin B12 forms on a modern column platform without the expensive requirement of an ultra-high pressure liquid chromatography and/or mass spectrometry. The method has a wide analytical range (0.0005% w/w - 85% w/w), high precision (repeatability relative standard deviations ranged from 1.08% to 3.06%), and high accuracy (>96% spike recovery rate). The method detection and quantification limits are less than 0.16 and 0.52 µg/mL, respectively. Conclusions To our best knowledge, the method is simpler, less time-consuming, and more economical than other published methods for its intended uses. Funding Sources Eurofins Supplement Analysis Center, Eurofins Scientific, Inc. MilliporeSigma Supporting Tables, Images and/or Graphs

The Three Rs in Research and Education: A Long Road Ahead in the United States

1996 ◽  
Vol 24 (2) ◽  
pp. 151-158 ◽  
Author(s):  
F. Barbara Orlans
Keyword(s):  
United States ◽  
Animal Experiments ◽  
The United States ◽  
Education Student ◽  
Funding Sources ◽  
Research And Education ◽  
The Right ◽  
Student Projects ◽  
Institutional Oversight ◽  
The Three Rs

Attitudes toward the Three Rs concept of refinement, reduction and replacement in the United States in research and education are widely divergent. Positive responses have come from several sources, notably from four centres established to disseminate information about alternatives. Funding sources to support work in the Three Rs have proliferated. The activities of institutional oversight committees have resulted in the nationwide implementation of important refinements. In the field of education, student projects involving pain or death for sentient animals have declined, and the right of students to object to participation in animal experiments on ethical grounds has been widely established. However, there is still a long way to go. Resistance to alternatives is deep-seated within several of the scientific disciplines most closely associated with animal research. The response of the National Institutes of Health to potentially important Congressional directives on the Three Rs has been unsatisfactory. The prestigious National Association of Biology Teachers, which at first endorsed the use of alternatives in education, later rescinded this policy, because of opposition to it. An impediment to progress is the extreme polarisation of viewpoints between the biomedical community and the animal protectionists.

scholarly journals Perspective: Characterization of Dietary Supplements Containing Calcium and Magnesium and Their Respective Ratio—Is a Rising Ratio a Cause for Concern?

2020 ◽  
Author(s):  
Rebecca B Costello ◽  
Andrea Rosanoff ◽  
Qi Dai ◽  
Leila G Saldanha ◽  
Nancy A Potischman
Keyword(s):  
Dietary Supplements ◽  
Total Mortality ◽  
The United States ◽  
Multiple Chronic Conditions ◽  
Range Data ◽  
Increased Risk ◽  
High Calcium ◽  
Liquid Products ◽  
Calcium And Magnesium ◽  
Ratio Range

ABSTRACT Low magnesium intakes coupled with high calcium intakes and high calcium-to-magnesium (Ca:Mg) intake ratios have been associated with increased risk for multiple chronic conditions such as cardiovascular disease and metabolic syndrome, as well as some cancers (colorectal, prostate, esophageal), and total mortality. A high dietary Ca:Mg ratio (>2.60) may affect body magnesium status while, on the other hand, high intakes of magnesium could adversely impact individuals with an exceedingly low dietary Ca:Mg ratio (<1.70). Thus, a Ca:Mg ratio range of 1.70–2.60 (weight to weight) has been proposed as an optimum range. Data from NHANES surveys have shown the mean Ca:Mg intake ratio from foods alone for US adults has been >3.00 since 2000. One-third of Americans consume a magnesium supplement with a mean dose of 146 mg/d, and 35% of Americans consume a calcium supplement with a mean dose of 479 mg/d. Our review of Ca:Mg ratios in dietary supplements sold in the United States and listed in NIH's Dietary Supplement Label Database (DSLD) found a mean ratio of 2.90 across all calcium- and magnesium-containing products, with differences by product form. The ratios ranged from a low of 0.10 in liquid products to a high of 48.5 in powder products. Thirty-one percent of products fell below, 40.5% fell within, and 28.3% fell above the ratio range of 1.70–2.60. Our findings of calculated Ca:Mg ratios from dietary supplements coupled with food-intake data suggest that, in individuals with high calcium intakes from diet and/or supplements, magnesium supplementation may be warranted to establish a more favorable dietary Ca:Mg ratio in their total diet. Additional research may provide greater insight into whether the Ca:Mg ratio is a biomarker of interest for moderating chronic disease and which population groups may derive benefit from moderating that ratio.

Response: The Use of Economic Anthropology in Economic Development

1995 ◽  
Vol 9 (4) ◽  
pp. 321-323
Author(s):  
Rhoda H. Halperin
Keyword(s):  
United States ◽  
Economic Development ◽  
Informal Economy ◽  
Analytical Methods ◽  
The United States ◽  
Development Research ◽  
Review Of The Literature ◽  
Street Vending ◽  
Research And Practice ◽  
History Of

The author comments on the use of anthropological methodologies in economic development research and practice in a developed economy such as the United States. The focus is the article by Morales, Balkin, and Persky on the closing of Chicago's Maxwell Street Market in August 1994. The article focuses on monetary losses for both buyers (consumers of market goods) and sellers (vendors of those goods) resulting from the closing of the market. Also included are a brief history of the market and a review of the literature on the informal economy. The authors measure “the value of street vending” by combining ethnographic and economic analytical methods.

scholarly journals Development and Validation of a Rapid RP-HPLC Method for the Estimation of Esmolol Hydrochloride in Bulk and Pharmaceutical Dosage Forms

2010 ◽  
Vol 7 (3) ◽  
pp. 807-812 ◽  
Author(s):  
Vanita Somasekhar ◽  
D. Gowri Sankar
Keyword(s):  
Limit Of Detection ◽  
Hplc Method ◽  
Detector Response ◽  
Reverse Phase Hplc ◽  
Limit Of Quantification ◽  
Pharmaceutical Dosage Forms ◽  
Rp Hplc ◽  
Accuracy And Precision ◽  
Development And Validation

A reverse phase HPLC method is described for the determination of esmolol hydrochloride in bulk and injections. Chromatography was carried on a C18column using a mixture of acetonitrile, 0.05 M sodium acetate buffer and glacial acetic acid (35:65:3 v/v/v) as the mobile phase at a flow rate of 1 mL/min with detection at 275 nm. The retention time of the drug was 4.76 min. The detector response was linear in the concentration of 1-50 μg/mL. The limit of detection and limit of quantification was 0.614 and 1.86 μg/mL respectively. The method was validated by determining its sensitivity, linearity, accuracy and precision. The proposed method is simple, economical, fast, accurate and precise and hence can be applied for routine quality control of esmolol hydrochloride in bulk and injections.

scholarly journals Development and Validation of UV Spectrophotometric Method for the Determination of Cefuroxime Axetil in Bulk and Pharmaceutical Formulation

2013 ◽  
Vol 6 (1) ◽  
pp. 133-141 ◽  
Author(s):  
S. Binte Amir ◽  
M. A. Hossain ◽  
M. A. Mazid
Keyword(s):  
Spectrophotometric Method ◽  
Cost Effective ◽  
Cefuroxime Axetil ◽  
Pharmaceutical Formulation ◽  
Uv Spectrum ◽  
Accuracy And Precision ◽  
Relative Standard ◽  
Label Claim ◽  
Development And Validation

The present study was undertaken to develop and validate a simple, sensitive, accurate, precise and reproducible UV spectrophotometric method for cefuroxime axetil using methanol as solvent. In this method the simple UV spectrum of cefuroxime axetil in methanol was obtained which exhibits absorption maxima (?max) at 278 nm. The quantitative determination of the drug was carried out at 278 nm and Beer’s law was obeyed in the range of (0.80-3.60) µg/ml. The proposed method was applied to pharmaceutical formulation and percent amount of drug estimated (95.6% and 96%) was found in good agreement with the label claim. The developed method was successfully validated with respect to linearity, specificity, accuracy and precision. The method was shown linear in the mentioned concentrations having line equation y = 0.05x + 0.048 with correlation coefficient of 0.995. The recovery values for cefuroxime axetil ranged from 99.85-100.05. The relative standard deviation of six replicates of assay was less than 2%. The percent relative standard deviations of inter-day precision ranged between 1.45-1.92% and intra-day precision of cefuroxime axetil was 0.96-1.51%. Hence, proposed method was precise, accurate and cost effective.  Keywords: UV-Vis spectrophotometer; Method validation; Cefuroxime axetil; Recovery studies.  © 2013 JSR Publications. ISSN: 2070-0237 (Print); 2070-0245 (Online). All rights reserved.   doi: http://dx.doi.org/10.3329/jsr.v6i1.14879 J. Sci. Res. 6 (1), 133-141 (2013)  

Evaluation of chemotherapy preparation processes: Volumetric method reliability and gravimetric method utility within 5 US hospitals

2021 ◽  
Author(s):  
Adam Moss ◽  
Stephanie Kang ◽  
Kathryn Morbitzer ◽  
Lam Nguyen ◽  
Moe Shwin ◽  
...  
Keyword(s):  
Gravimetric Method ◽  
The United States ◽  
Volumetric Method ◽  
Preparation Process ◽  
Accuracy And Precision ◽  
Data Collection Process ◽  
Accurate Dose ◽  
Actual Volume ◽  
Drug Expenditures ◽  
Transfer Device

Abstract Disclaimer In an effort to expedite the publication of articles , AJHP is posting manuscripts online as soon as possible after acceptance. Accepted manuscripts have been peer-reviewed and copyedited, but are posted online before technical formatting and author proofing. These manuscripts are not the final version of record and will be replaced with the final article (formatted per AJHP style and proofed by the authors) at a later time. Purpose The primary aim of this study was to investigate the accuracy of the volumetric method for intravenous (IV) preparations and explore the utility of gravimetric methods in the medication preparation process within multiple institutions. Secondary outcomes of this study were syringe size percent variations and impact on drug expenditures. Methods A prospective, noninterventional, multisite study was conducted between March 2015 and December 2016 to generate baseline estimates of accuracy and precision in the volumetric medication preparation process. Five hospitals in the United States were recruited for study participation. During the data collection process, technicians were required to measure the syringe at 3 different points: when the new empty syringe was connected to a closed-system transfer device (CSTD), when the filled syringe containing the prepared dose of medication was connected to a CSTD, and when the used syringe with residual medication was connected to a CSTD. The actual dose of drug dispensed (in mg) was divided by the specific gravity of the medication to determine the actual volume of medication dispensed. Results A total of 4,443 compounded sterile products representing 60 medications across 5 hospitals were eligible for the study. Of the evaluated preparations, 91.92% were within 5% of the prescribed dose and 96.56% were within 10% of the prescribed dose. The outliers ranged from –144.10% to 233.72%. Conclusion The potential for significant over- and undertreatment of an individual patient receiving IV chemotherapy exists, indicating the need for an additional measurement method, such as real-time gravimetric verification, to ensure an accurate dose is administered to every patient.

VALIDATED RP-HPLC AND UV-SPECTROSCOPY METHODS FOR THE ESTIMATION OF DAPAGLIFLOZIN IN BULK AND IN TABLETS

INDIAN DRUGS ◽  
2017 ◽  
Vol 54 (03) ◽  
pp. 44-51
Author(s):  
B. Sabbagh ◽  
B. V. S. Lokesh ◽  
G. A. Akouwah ◽  
Keyword(s):  
Good Accuracy ◽  
Uv Spectroscopy ◽  
Linear Regression Analysis ◽  
Molar Absorptivity ◽  
Hplc Method ◽  
Rp Hplc ◽  
Accuracy And Precision ◽  
Significant Difference ◽  
Uv Visible

Two methods were developed for the determination of dapagliflozin (DAPA) in pure form and in tablets. The procedure utilized was UV-Visible Spectroscopy and RP-HPLC with PDA detector to quantify DAPA in bulk and tablets. The sensitive linear range was identified for both methods within 0.5-5.0μg/mL. The linear regression analysis was identified for both methods with correlation coefficient(r)>0.99. The LOD and LOQ values were found to be 0.05 μg/mL and 0.5 μg/mL for the method by UV-Spectroscopy. The molar absorptivity (ε) was calculated as 1.27 X 105 L.mol-1cm-1. The RP-HPLC method produced LOD and LOQ values of 1.0 ng/mL and 0.5 μg/mL. Both methods were simple, precise, reproducible to quantify the amount of unknown in bulk as well as in tablets and estimated accurately within the range of 100.0±0.5%. Statistical analysis was performed on the data obtained. There was no significant difference between the developed and reported methods with p>0.05. Both methods can be applied for routine analysis of DAPA in bulk and tablets with good accuracy and precision.

Considerations in the preparation of laboratory samples for the analysis of ochratoxin A in wheat

2012 ◽  
Vol 5 (2) ◽  
pp. 107-116 ◽  
Author(s):  
S.A. Tittlemier ◽  
M. Roscoe ◽  
C. Kobialka ◽  
R. Blagden
Keyword(s):  
Ochratoxin A ◽  
Whole Grain ◽  
Laboratory Sample ◽  
Test Portion ◽  
Homogeneous Sample ◽  
Ambient Temperatures ◽  
Accuracy And Precision ◽  
Relative Standard ◽  
The Mean ◽  
Ground Wheat

A process used to prepare the test portion of ground wheat from the whole grain laboratory sample for ochratoxin A (OTA) analysis using dry comminution with homogenisation and sub-sampling via a rotary sample divider was developed and evaluated. With respect to OTA content, the developed process produced a homogeneous sample of ground wheat from 10 kg of whole grain. Relative standard deviations of the mean OTA concentration for five naturally contaminated wheat samples processed using the developed method ranged from 9% to 19% over a relevant concentration range of 1.7 to 7.6 mg/kg. Additional studies demonstrated that OTA was stable in ground wheat with moisture content between 12 to 13% for at least a year when stored at ambient temperatures. Further examination of the developed comminution and dividing procedure demonstrated that higher concentrations were measured in smaller sized particles, indicating that the accuracy and precision of OTA analyses could be affected by the particle size of ground wheat.

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