scholarly journals Intra-Laboratory Validation of Alpha-Galactosidase Activity Measurement in Dietary Supplements

Molecules ◽  
2021 ◽  
Vol 26 (6) ◽  
pp. 1566
Author(s):  
Elena Fabris ◽  
Michela Bulfoni ◽  
Alessandro Nencioni ◽  
Emanuele Nencioni
Keyword(s):  
Dietary Supplements ◽  
Good Manufacturing Practice ◽  
Activity Measurement ◽  
Intermediate Precision ◽  
Method Performance ◽  
Intestinal Gas ◽  
Technical Requirements ◽  
Ich Guidelines ◽  
Alpha Galactosidase

Introduction: Alpha-galactosidase (α-Gal) is an enzyme responsible for the hydrolyzation of glycolipids and glycoprotein commonly found in dietary sources. More than 20% of the general population suffers from abdominal pain or discomfort caused by intestinal gas and by indigested or partially digested food residuals. Therefore, α-Gal is used in dietary supplements to reduce intestinal gases and help complex food digestion. Marketed enzyme-containing dietary supplements must be produced in accordance with the Food and Drug Administration (FDA) regulations for Current Good Manufacturing Practice (cGMPs). Aim: in this work we illustrated the process used to develop and validate a spectrophotometric enzymatic assay for α-Gal activity quantification in dietary supplements. Methods: The validation workflow included an initial statistical-phase optimization of materials, reagents, and conditions, and subsequently a comparative study with another fluorimetric assay. A final validation of method performance in terms of specificity, linearity, accuracy, intermediate-precision repeatability, and system precision was then executed. Results and conclusions: The proven method achieved good performance in the quantitative determination of α-Gal activity in commercial food supplements in accordance with the International Council for Harmonisation of Technical Requirements for Pharmaceuticals (ICH) guidelines and is suitable as a rapid in-house quality control test.

scholarly journals Determination of Chondroitin Sulfate Content in Raw Materials and Dietary Supplements by High-Performance Liquid Chromatography with UV Detection After Enzymatic Hydrolysis: Single-Laboratory Validation First Action 2015.11

2016 ◽  
Vol 99 (1) ◽  
pp. 53-54
Author(s):  
Sharon L Brunelle
Keyword(s):  
Chondroitin Sulfate ◽  
Dietary Supplements ◽  
High Performance ◽  
Raw Materials ◽  
Method Performance ◽  
Expert Review ◽  
Performance Requirements ◽  
Expert Review Panel ◽  
Single Laboratory

Abstract A previously validated method for determination of chondroitin sulfate in raw materials and dietary supplements was submitted to the AOAC Expert Review Panel (ERP) for Stakeholder Panel on Dietary Supplements Set 1 Ingredients (Anthocyanins, Chondroitin, and PDE5 Inhibitors) for consideration of First Action Official MethodsSM status. The ERP evaluated the single-laboratory validation results against AOAC Standard Method Performance Requirements 2014.009. With recoveries of 100.8–101.6% in raw materials and 105.4–105.8% in finished products and precision of 0.25–1.8% RSDr within-day and 1.6–4.72% RSDr overall, the ERP adopted the method for First Action Official Methods status and provided recommendations for achieving Final Action status.

Determination of Sodium Fluoroacetate in Dairy Powders by Liquid Chromatography–Tandem Mass Spectrometry: Single-Laboratory Validation, First Action 2015.02

2016 ◽  
Vol 99 (1) ◽  
pp. 242-251 ◽  
Author(s):  
Lauren M Fleury ◽  
Bryan G Scahill ◽  
Rilka Taskova
Keyword(s):  
Infant Formula ◽  
Intermediate Precision ◽  
Method Performance ◽  
Expert Review ◽  
Liquid Chromatography Tandem Mass ◽  
Expert Review Panel ◽  
Single Laboratory ◽  
Lc Tandem Ms ◽  
Dairy Powders

Abstract A single-laboratory validation (SLV) study was conducted for the determination of sodium fluoroacetate in dairy powders by LC-tandem MS (LC-MS/MS). Linearity of response was confirmed by analysis of samples fortified over the concentration range 0.10–100 μg/kg. The LOD was estimated to be 0.028 μg/kg (0.028 ppb) from the SD of the measured concentrations of infant formula samples fortified at 0.10 μg/kg. The corresponding LOQ calculates at 0.085 μg/kg (0.085 ppb), which ensures excellent reliability of quantification at the limit of reporting of 1.0 μg/kg (1 ppb). Repeatability and intermediate precision were estimated from the SD of the recovery of samples fortified at 0.075, 0.10, 0.20, 0.50, 1.0, and 10.0 μg/kg. The previously mentioned method performance values were established using a representative stage 2 (6–12 months) bovine infant formula, and the robustness of the method was tested by the analysis of 107 unique dairy powders and formulations fortified at 1.0 μg/kg. The data collected in this study satisfy the requirements of SLV studies established by the AOAC Stakeholder Panel on Infant Formula and Adult Nutritionals (SPIFAN), and the method was awarded First Action Official MethodSM status by the AOAC Expert Review Panel on SPIFAN Nutrient Methods (Contaminants) on March 17, 2015.

scholarly journals Validated RP-HPLC Method for the Determination of Ivabradine Hydrochloride in Pharmaceutical Formulation

2017 ◽  
Vol 9 (05) ◽  
Author(s):  
MD. Muzaffar -ur- Rehman1 ◽  
G. Nagamallika
Keyword(s):  
Mobile Phase ◽  
Dosage Forms ◽  
Hplc Method ◽  
Pharmaceutical Formulation ◽  
Intermediate Precision ◽  
Pharmaceutical Dosage Forms ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
Bulk Drug

A simple, rapid, precise, and accurate RP-HPLC method for the estimation of Ivabradine Hydrochloride an anti-anginal agent, both as a bulk drug and in pharmaceutical formulation was developed. The chromatographic separation was achieved on a Thermosil C18 150 × 4.5 mm, 5μm column by using a mobile phase containing a mixture of methanol and phosphate buffer pH 6.5 in the ratio of 65:35 % v/v at a flow rate of 1ml/min and at an ambient temperature. The detection was monitored at a wavelength of 265nm. A clear chromatographic peak was identified with the retention time of 4.36 min and tailing factor of 1.23. The developed method was validated according to ICH guidelines with respect to specificity, linearity, accuracy, precision and robustness. The method shows a good linear relationship with correlation co-efficient of more than 0.992 in the concentration range of 30μg-150μg. The method showed mean % Recovery of 100.4% and %RSD for repeatability and intermediate precision was less than 2%. The proposed method can be used successfully for the quantitative determination of Ivabradine HCL in pharmaceutical dosage forms.

Validation of the framycetin sulfate determination technique by HPLC in a Framidex medicinal preparation

2020 ◽  
Vol 86 (6) ◽  
pp. 73-78
Author(s):  
D. D. Gapparov ◽  
Z. A. Smanova ◽  
Y. V. Timchenko ◽  
A. V. Pirogov
Keyword(s):  
Medicinal Preparation ◽  
Good Manufacturing Practice ◽  
Variation Coefficient ◽  
Intermediate Precision ◽  
Average Value ◽  
Limit Of Determination ◽  
Validation Criteria ◽  
Derivatizing Agent ◽  
Order Of Magnitude

A method for determination of framycetin sulfate in a Framidex preparation (eye and ear drops) by HPLC-UV (λ = 365 nm) using 2, 4-dinitrofluorobenzene as a derivatizing agent has been developed The characteristics of analytical methods determined for the purpose of their validation and relevant criteria for the validity of validated methods with the goal of the quality control of drugs (pharmaceutical substances and drugs) are presented. According to the results of an intralaboratory experiment on the validation assessment of the method by the parameters of the specificity, limit of determination (LOD), linearity, precision and laboratory accuracy, it is shown that the LOD decreases by an order of magnitude, the correlation coefficient is not less than 0.99 correctness (average value — 97.5 – 102.5%; variation coefficient — not more than 2.0%; the confidence range should include 100% of values), convergence (variation coefficient — not more than 1.5%), intermediate precision (variation coefficient — not more than 1.5%). It is shown that the obtained values of metrological characteristics do not exceed the validation criteria and the developed method matches all the well-known requirements of GMP (Good Manufacturing Practice).

Determination of Vitamin K1 in Infant, Pediatric, and Adult Nutritionals by HPLC with Fluorescence Detection: Single-Laboratory Validation, First Action 2015.09

2015 ◽  
Vol 98 (5) ◽  
pp. 1382-1389 ◽  
Author(s):  
Mary Bidlack ◽  
Linda D Butler Thompson ◽  
Wesley A Jacobs ◽  
Karen J Schimpf
Keyword(s):  
Fluorescence Detection ◽  
Hplc Method ◽  
Excitation Wavelength ◽  
Vitamin K1 ◽  
Intermediate Precision ◽  
Method Performance ◽  
Performance Requirements ◽  
Normal Phase Hplc ◽  
Single Laboratory

Abstract This normal-phase HPLC method with postcolumn reduction and fluorescence detection allows for the quantitative determination of trans vitamin K1 in infant, pediatric, and adult nutritionals. Vitamin K1 is extracted from products with iso-octane after precipitation of proteins and release of lipids with methanol. Prepared samples are injected onto a silica HPLC column where cis and trans vitamin K1 are separated with an iso-octane–isopropanol mobile phase. The column eluent is mixed with a dilute ethanolic solution of zinc chloride, sodium acetate, and acetic acid, and vitamin K1 is reduced to a fluorescent derivative in a zinc reactor column. The resulting hydroquinone is then detected by fluorescence at an excitation wavelength of 245 nm and an emission wavelength of 440 nm. During a single-laboratory validation of this method, repeatability and intermediate precision ranged from 0.6 to 3.5% RSD and 1.1 to 6.0% RSD, respectively. Mean overspike recoveries ranged from 91.9 to 106%. The method demonstrated good linearity over a standard range of approximately 2–90 μg/L trans vitamin K1 with r2 averaging 0.99995 and average calibration errors of <1%. LOQ and LOD in ready-to-feed nutritionals were estimated to be 0.03 and 0.09 μg/100 g, respectively. The method met AOAC Stakeholder Panel on Infant Formula and Adult Nutritionals Standard Method Performance Requirements® and was approved as a first action method at the 2015 AOAC Mid-Year Meeting.

Determination of Fructans in Infant, Adult, and Pediatric Nutritional Formulas: Single-Laboratory Validation, First Action 2016.06

2016 ◽  
Vol 99 (6) ◽  
pp. 1576-1588 ◽  
Author(s):  
Philip Haselberger ◽  
Wesley A Jacobs
Keyword(s):  
Quantitative Analysis ◽  
Sample Preparation ◽  
Profile Analysis ◽  
Correction Factors ◽  
Intermediate Precision ◽  
Size Category ◽  
Method Performance ◽  
Performance Requirements ◽  
Single Laboratory

Abstract A method for fructan analysis designed to comply with AOAC Standard Method Performance Requirements (SMPR®) 2014.002 is described. It is closely related to existing methods for fructan analysis, including AOAC 997.08 and 999.03, as well as a method previously published by Cuany et al. This new method achieves LOQ of 0.03% fructan on a ready-to-feed (RTF) basis with mean recoveries ranging from 93 to 108% in the presence of up to 9% sucrose (even at the 0.03% level of fructan). Repeatability ranged from 1.09 to 3.67%. Intermediate precision ranged from 2.46 to 6.79%. Sample preparation for quantitative analysis is simplified compared to some of the existing methodologies. The method incorporates a qualitative profile analysis to determine fructan size category. This allows assignment of appropriate correction factors without independent knowledge of fructan type.

scholarly journals Validated stability indicating RP-HPLC method for the determination of dolutegravir and rilpivirine in bulk and pharmaceutical dosage forms

2021 ◽  
Vol 12 (3) ◽  
pp. 1961-1966
Author(s):  
Gopinath K ◽  
Padmavathi K. V. ◽  
Murali Krishna N ◽  
Subbarao M
Keyword(s):  
Drug Testing ◽  
Orthophosphoric Acid ◽  
Hplc Method ◽  
Intermediate Precision ◽  
Pharmaceutical Dosage Forms ◽  
Rp Hplc ◽  
Acceptable Range ◽  
Ich Guidelines ◽  
Ethyl Amine

For simultaneous analysis of Dolutegravir and Rilpivirine utilizing RP-HPLC, an accurate, rapid, economical, quick and reliable assay technique was developed and tested. Successful chromatographic detachment using acetonitrile and 0.1 percent tri ethyl amine in the water of pH-2.5 adjusted with 0.1% orthophosphoric acid in 40:60 v/v as a movable phase with a flow of 1 ml/min and UV observation at 230 nm. Chromatography at ambient temperature was performed isocratically, and the run time was 10 min. By injecting the norm six times, device suitability parameters were studied and the findings were far below the acceptance criteria. The linearity analysis was performed at levels ranging from 10% to 150% and the R2 value was found to be 0.999. Precision has been found to be 0.8 for repeatability and 1.2 for intermediate precision. Assay of the commercialized formulation was performed by using the above method, and we get 100.01 percent was present. For routine analysis in drug testing, this chromatographic approach can be effectively implemented. By using the above technique, an assay of the marketed formulation was performed and found to be within the limit. Degradation studies were carried out on Dolutegravir and Rilpivirine, with a purity threshold greater than purity angle in all conditions and within the acceptable range. The above-mentioned technique was validated according to ICH guidelines. 

Simultaneous Determination of Vitamins D2 and D3 by LC-MS/MS in Infant Formula and Adult Nutritionals: First Action 2011.13

2012 ◽  
Vol 95 (3) ◽  
pp. 583-587 ◽  
Author(s):  
Donald L Gilliland ◽  
Charles K Black ◽  
James E Denison ◽  
Charles T Seipelt ◽  
Dawn Dowell
Keyword(s):  
Simultaneous Determination ◽  
Infant Formula ◽  
Practical Method ◽  
Intermediate Precision ◽  
Method Performance ◽  
Expert Review ◽  
Performance Requirements ◽  
Expert Review Panel ◽  
Working Standards

Abstract During the “Standards Development and International Harmonization: AOAC INTERNATIONAL Mid-Year Meeting” held on June 29, 2011, an Expert Review Panel (ERP) on behalf of AOAC INTERNATIONAL adopted the method “Simultaneous Determination of Vitamins D2 and D3 by LC-MS/MS in Infant Formula and Adult Nutritionals” as an AOAC Official First Action method. Vitamins D2 and D3 are extracted from the sample using pentane–ether; the extract is collected and dried under nitrogen. Vitamin D is separated from interfering compounds using UPLC, and quantitated using tandem mass spectrometry (MS/MS). Preliminary data showed the intermediate precision ranged from 3.34–8.05% and an accuracy range of 98.5–111% over the samples tested for vitamin D3. For vitamin D2, the intermediate precision ranged from 2.37–5.45% and accuracy ranged from 96.4–104% over the four matrixes evaluated. The analytical range for the method is bounded by the concentrations of the working standards, 21–270 ng/mL, and is equivalent to 0.168–2.16 mcg/100 g in ready-to-feed product. The practical method quantitation limit is 0.168 mcg/100 g product with method detection limit of 60 ng/100 g product. The ERP reviewed the data and determined that the performance characteristics of the method met the standard method performance requirements, and therefore the method was granted First Action status.

scholarly journals Development and Validation of UV Spectrophotometric Method For Determination of Bisoprolol Fumarate in Bulk and Pharmaceutical Dosage Forms

2017 ◽  
Vol 6 (5) ◽  
pp. 196-199 ◽  
Author(s):  
Shahinaz Mohammed ◽  
Mohammed Adam ◽  
Shaza Shantier
Keyword(s):  
Spectrophotometric Method ◽  
Limit Of Detection ◽  
Limit Of Quantification ◽  
Intermediate Precision ◽  
Pharmaceutical Dosage Forms ◽  
Ich Guidelines ◽  
Recovery Percentage ◽  
Development And Validation ◽  
Tablet Dosage

In this study a simple, accurate and precise UV- spectrophotometric method was developed for the estimation of bisoprolol fumarate (BF) in bulk and tablet dosage form. The method was based on measurement of absorbance of BF aqueous solution at 271nm. Validation was conducted in accordance to ICH guidelines. The calibration curve was linear in the concentration range 5-25 µg/mL with correlation coefficient not less than 0.9986. The limit of detection and limit of quantification were 0.22 μg/ml and 0.66 μg/ml, respectively. Intraday and intermediate precision of the developed method were reflected by the low RSD% values (1.19 and 0.854, respectively). The recovery percentage was 105.0 ± 1.3%, n=3. The proposed method was applied for the assay of BF in three different brands

Method for the Determination of Lycopene in Supplements and Raw Material by Reversed-Phase Liquid Chromatography: Single-Laboratory Validation

2008 ◽  
Vol 91 (6) ◽  
pp. 1284-1297 ◽  
Author(s):  
André Müller ◽  
Bernd Pietsch ◽  
Nicole Faccin ◽  
Joseph Schierle ◽  
Edward H Waysek
Keyword(s):  
Dietary Supplements ◽  
High Performance ◽  
Raw Materials ◽  
Reversed Phase ◽  
Raw Material ◽  
Intermediate Precision ◽  
Relative Standard ◽  
Product Forms ◽  
Single Laboratory

Abstract A single-laboratory validation study was conducted for a liquid chromatographic (LC) method for the determination of total and all-trans-lycopene in a variety of dietary supplements and raw materials. Gelatin-based and other water-dispersible beadlets, or tablets, capsules, and softgels containing such product forms, were digested with protease. Alginate formulations and the respective applications were treated with an alkaline sodium EDTA acetate buffer to release lycopene from the matrix. Lycopene and other carotenoids were extracted from the resulting aqueous suspensions with dichloromethane and ethanol. Oily product forms were directly dissolved in dichloromethane and ethanol. The extracts were chromatographed on an isocratic high-performance LC system using a C16 alkylamide modified silica column that provided satisfactory resolution of all-trans-lycopene from its predominant cis-isomers and separated the lycopene isomers from other carotenoids such as - and -carotene, cryptoxanthin, lutein, and zeaxanthin. The within-day precision relative standard deviation (RSD) for the determination of total lycopene ranged from 0.9 to 5.7 over concentration ranges of 50200 g/kg for raw materials and 0.324 g/kg for dietary supplements. The intermediate precision RSD (total RSD) ranged from 0.8 to 8.9. Recoveries obtained for beadlet and tablet material for the different extraction variants ranged from 95.0 to 102.1 at levels of 0.0220 g/kg for tablets and from 95.0 to 101.1 at levels of 1200 g/kg for beadlet material.

Sign in / Sign up

Export Citation Format

Share Document