Fractional factorial experiments using a test atmosphere to assess the accuracy and precision of a new passive sampler for the determination of formaldehyde in the atmosphere

Aim and scope: Due to the serious toxicological risks and their widespread use, quantitative determination of phthalates in cosmetic products have importance for public health. The aim of this study was to develop a validated simple, rapid and reliable high-performance liquid chromatography (HPLC) method for the determination of phthalates which are; dimethyl phthalate (DMP), diethyl phthalate (DEP), benzyl butyl phthalate (BBP), di-n-butyl phthalate (DBP), di(2- ethylhexyl) phthalate (DEHP), in cosmetic products and to investigate these phthalate (PHT) levels in 48 cosmetic products marketing in Sivas, Turkey. Materials and Methods: Separation was achieved by a reverse-phase ACE-5 C18 column (4.6 x 250 mm, 5.0 μm). As the mobile phase, 5 mM KH2PO4 and acetonitrile were used gradiently at 1.5 ml min-1. All PHT esters were detected at 230 nm and the run time was taking 21 minutes. Results: This method showed the high sensitivity value the limit of quantification (LOQ) values for which are below 0.64 μg mL-1 of all phthalates. Method linearity was ≥0.999 (r2). Accuracy and precision values of all phthalates were calculated between (-6.5) and 6.6 (RE%) and ≤6.2 (RSD%), respectively. Average recovery was between 94.8% and 99.6%. Forty-eight samples used for both babies and adults were successfully analyzed by the developed method. Results have shown that, DMP (340.7 μg mL-1 ±323.7), DEP (1852.1 μg mL-1 ± 2192.0), and DBP (691.3 μg mL-1 ± 1378.5) were used highly in nail polish, fragrance and cream products, respectively. Conclusion: Phthalate esters, which are mostly detected in the content of fragrance, cream and nail polish products and our research in general, are DEP (1852.1 μg mL-1 ± 2192.0), DBP (691.3 μg mL-1 ± 1378.5) and DMP (340.7 μg mL-1 ±323.7), respectively. Phthalates were found in the content of all 48 cosmetic products examined, and the most detected phthalates in general average were DEP (581.7 μg mL-1 + 1405.2) with a rate of 79.2%. The unexpectedly high phthalate content in the examined cosmetic products revealed a great risk of these products on human health. The developed method is a simple, sensitive, reliable and economical alternative for the determination of phthalates in the content of cosmetic products, it can be used to identify phthalate esters in different products after some modifications.

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Recent Applications of High Performance Thin Layer Chromatography and Derivative Spectrophotometry in Pharmaceutical Analysis

Current Pharmaceutical Analysis ◽

10.2174/1573412915666190226155149 ◽

2020 ◽

Vol 16 (6) ◽

pp. 671-689

Author(s):

Marcin Gackowski ◽

Marcin Koba ◽

Katarzyna Mądra-Gackowska ◽

Piotr Kośliński ◽

Stefan Kruszewski

Keyword(s):

Thin Layer ◽

Thin Layer Chromatography ◽

Pharmaceutical Analysis ◽

High Performance ◽

Degradation Products ◽

Derivative Spectrophotometry ◽

Accuracy And Precision ◽

Post Marketing ◽

Layer Chromatography

At present, no one can imagine drug development, marketing and post-marketing without rigorous quality control at each stage. Only modern, selective, accurate and precise analytical methods for determination of active compounds, their degradation products and stability studies are able to assure the appropriate amount and purity of drugs administered every day to millions of patients all over the world. For routine control of drugs simple, economic, rapid and reliable methods are desirable. The major focus of current scrutiny is placed on high-performance thin layer chromatography and derivative spectrophotometry methods, which fulfill routine drug estimation’s expectations [1-4]. The present paper reveals state-of-the-art and possible applications of those methods in pharmaceutical analysis between 2010 and 2018. The review shows advantages of high-performance thin layer chromatography and derivative spectrophotometry, including accuracy and precision comparable to more expensive and time-consuming methods as well as additional fields of possible applications, which contribute to resolving many analytical problems in everyday laboratory practice.

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A Green Liquid Chromatographic Method For The Simultaneous Determination of Chlorpheniramine Maleate, Pseudoephedrine Hydrochloride and Propyphenazone

Current Analytical Chemistry ◽

10.2174/1573411014666180806155002 ◽

2019 ◽

Vol 15 (6) ◽

pp. 635-641

Author(s):

Nadia M. Mostafa ◽

Ghada M. Elsayed ◽

Nagiba Y. Hassan ◽

Dina A. El Mously

Keyword(s):

Simultaneous Determination ◽

Mobile Phase ◽

Dosage Form ◽

Chromatographic Method ◽

Green Analytical Chemistry ◽

Chlorpheniramine Maleate ◽

Accuracy And Precision ◽

Liquid Chromatographic Method ◽

Liquid Chromatographic

Background:The concept of green analytical chemistry prevails due to the growing environmental pollution.Objective:Our attempts are to develop simple and eco-friendly method which is non-harmful to the environment by producing minimal waste. In this context, a green liquid chromatographic method was applied for the simultaneous determination of chlorpheniramine maleate, pseudoephedrine hydrochloride and propyphenazone in their combined dosage form.Methods:Separation was carried out using X select HSS RP C18 analytical column (250 × 4.6 mm, 5μm) using methanol - 0.02 M phosphate buffer pH 3 - triethylamine (60:40: 0.1, by volume) as a mobile phase. The separated peaks were detected at 215 nm at a flow rate 1.0 mL/min.Results:Quantification was done over the concentration ranges of 1-25 µg/mL for chlorpheniramine maleate, 5-35 µg/mL for pseudoephedrine hydrochloride and 10-120 µg/mL for propyphenazone. The suggested method was validated with regard to linearity, accuracy and precision according to the International Conference on Harmonization guidelines with good results.Conclusion:It could be used as a safer alternative for routine analysis of the mentioned drugs in quality control laboratories.

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A Rapid Method for Determination of Buprenorphine and Norbuprenorphine in Urine by UPLC-MS/MS

Current Pharmaceutical Analysis ◽

10.2174/1573412916999200627010536 ◽

2020 ◽

Vol 16 ◽

Author(s):

Aykut Kul ◽

Murat Ozdemir ◽

Selma Ozilhan ◽

Olcay Sagirli

Keyword(s):

Forensic Science ◽

Rapid Method ◽

Proficiency Testing ◽

Mass Spectrometer ◽

Illicit Market ◽

Analysis Methods ◽

Accuracy And Precision ◽

Lower Limits

Background: Buprenorphine is quite common in the illicit market. Buprenorphine-containing drugs abuse is frequently encountered in patients. The analysis methods used to determine the abuse of buprenorphine and norbuprenorphine are important for forensic science. Buprenorphine is metabolized to norbuprenorphine by the liver. Objective: Therefore, the determination of buprenorphine and norbuprenorphine in urine is one of the methods to determine the abuse of buprenorphine. Methods: In this study, we have developed a precise, simple, and rapid ultra-performance liquid chromatographytandem mass spectrometer method for the determination of buprenorphine and norbuprenorphine simultaneously. Results: The developed method was validated in terms of selectivity and linearity, which was in the range of 9–1800 ng/mL for both buprenorphine and norbuprenorphine. The intra-assay and inter-assay accuracy and precision were found within acceptable limits of the EMA guideline. Lower limits of quantitation were 9 ng/mL for both buprenorphine and norbuprenorphine. Conclusion: The developed method was successfully applied for the determination of both analytes in the proficiency testing samples.

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Simplified and Rapid Determination of Primaquine and 5,6-Orthoquinone Primaquine by UHPLC-MS/MS: Its Application to a Pharmacokinetic Study

Molecules ◽

10.3390/molecules26144357 ◽

2021 ◽

Vol 26 (14) ◽

pp. 4357

Author(s):

Waritda Pookmanee ◽

Siriwan Thongthip ◽

Jeeranut Tankanitlert ◽

Mathirut Mungthin ◽

Chonlaphat Sukasem ◽

...

Keyword(s):

Pharmacokinetic Study ◽

High Performance ◽

Rapid Determination ◽

Active Metabolites ◽

Chromatography Tandem Mass Spectrometry ◽

Accuracy And Precision ◽

The Matrix ◽

Liquid Chromatography Tandem Mass ◽

Isocratic Mode

The method for the determination of primaquine (PQ) and 5,6-orthoquinone primaquine (5,6-PQ), the representative marker for PQ active metabolites, via CYP2D6 in human plasma and urine has been validated. All samples were extracted using acetonitrile for protein precipitation and analyzed using the ultra-high-performance liquid chromatography–tandem mass spectrometry (UHPLC-MS/MS) system. Chromatography separation was carried out using a Hypersil GOLDTM aQ C18 column (100 × 2.1 mm, particle size 1.9 μm) with a C18 guard column (4 × 3 mm) flowed with an isocratic mode of methanol, water, and acetonitrile in an optimal ratio at 0.4 mL/min. The retention times of 5,6-PQ and PQ in plasma and urine were 0.8 and 1.6 min, respectively. The method was validated according to the guideline. The linearity of the analytes was in the range of 25–1500 ng/mL. The matrix effect of PQ and 5,6-PQ ranged from 100% to 116% and from 87% to 104% for plasma, and from 87% to 89% and from 86% to 87% for urine, respectively. The recovery of PQ and 5,6-PQ ranged from 78% to 95% and form 80% to 98% for plasma, and from 102% to from 112% to 97% to 109% for urine, respectively. The accuracy and precision of PQ and 5,6-PQ in plasma and urine were within the acceptance criteria. The samples should be kept in the freezer (−80 °C) and analyzed within 7 days due to the metabolite stability. This validated UHPLC-MS/MS method was beneficial for a pharmacokinetic study in subjects receiving PQ.

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Comparative Study for the Assay of Plant Derived Chemicals in Pharmaceutical Formulation Using Methods Dependent on Factorized Spectra

Journal of AOAC International ◽

10.1093/jaoacint/qsab027 ◽

2021 ◽

Author(s):

Nesma M Fahmy ◽

Adel M Michael

Keyword(s):

Pharmaceutical Formulations ◽

Pharmaceutical Formulation ◽

Ternary Mixtures ◽

Ratio Method ◽

The Novel ◽

Naturally Occurring ◽

Accuracy And Precision ◽

Validation Parameters ◽

Significant Difference

Abstract Background Modern built-in spectrophotometer software supporting mathematical processes provided a solution for increasing selectivity for multicomponent mixtures. Objective Simultaneous spectrophotometric determination of the three naturally occurring antioxidants—rutin(RUT), hesperidin(HES), and ascorbic acid(ASC)—in bulk forms and combined pharmaceutical formulation. Method This was achieved by factorized zero order method (FZM), factorized derivative method (FD1M), and factorized derivative ratio method (FDRM), coupled with spectrum subtraction(SS). Results Mathematical filtration techniques allowed each component to be obtained separately in either its zero, first, or derivative ratio form, allowing the resolution of spectra typical to the pure components present in Vitamin C Forte® tablets. The proposed methods were applied over a concentration range of 2–50, 2–30, and 10–100 µg/mL for RUT, HES, and ASC, respectively. Conclusions Recent methods for the analysis of binary mixtures, FZM and FD1M, were successfully applied for the analysis of ternary mixtures and compared to the novel FDRM. All were revealed to be specific and sensitive with successful application on pharmaceutical formulations. Validation parameters were evaluated in accordance with the International Conference on Harmonization guidelines. Statistical results were satisfactory, revealing no significant difference regarding accuracy and precision. Highlights Factorized methods enabled the resolution of spectra identical to those of pure drugs present in mixtures. Overlapped spectra of ternary mixtures could be resolved by spectrum subtraction coupled FDRM (SS-FDRM) or by successive application of FZM and FD1M.

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Spectrophotometric determination of dothiepin hydrochloride in pharmaceuticals through ion-pair complexation reaction

Chemical Industry and Chemical Engineering Quarterly ◽

10.2298/ciceq111009010a ◽

2012 ◽

Vol 18 (2) ◽

pp. 339-347 ◽

Cited By ~ 4

Author(s):

Sameer Abdulrahman ◽

Kanakapura Basavaiah

Keyword(s):

Ion Pair ◽

Pure Form ◽

Bromocresol Green ◽

Bromophenol Blue ◽

Complexation Reaction ◽

Conditional Stability ◽

Conditional Stability Constant ◽

Accuracy And Precision ◽

Significant Difference

Two simple, sensitive and extraction-free spectrophotometric methods are described for the determination of dothiepin hydrochloride (DOTH) both in pure form and in pharmaceutical tablets. The methods are based on ion-pair complex formation between dothiepin base (DOT) and two acidic dyes, namely, bromophenol blue (BPB) or bromocresol green (BCG) with absorption maximum at 425 nm for BPB method or 430 nm for BCG method. Beer?s law is obeyed over the concentration ranges of 1.0-15.0 and 1.0-17.5 ?g mL-1 DOT for BPB and BCG methods, respectively. The molar absorptivity values and Sandell?s sensitivity values are reported for both methods. The limits of detection (LOD) and quantification (LOQ) were calculated to be 0.18 and 0.53 ?g mL-1 for BPB method, and 0.17 and 0.50 ?g mL-1 for BCG method, respectively. The stoichiometry of the complex in either case was found to be 1: 1 and the conditional stability constant (KF) of the complexes has also been calculated. The proposed methods were applied successfully to the determination of DOTH in pure form and in its tablet form with good accuracy and precision. Statistical comparison of the results was performed using Student's t-test and variance ratio F-test at 95% confidence level and there was no significant difference between the official and proposed methods with regard to accuracy and precision. Further, the validity of the proposed methods was confirmed by recovery studies via standard addition technique.

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Assessment and determination of lyoprotectant for survival of freeze-dried Lactobacillus rhamnosus

Acta Universitatis Cibiniensis Series E Food Technology ◽

10.1515/aucft-2016-0009 ◽

2016 ◽

Vol 20 (1) ◽

pp. 105-113

Author(s):

Zongcheng Miao ◽

Yang Zhao ◽

Xiaoping Huo

Keyword(s):

Amino Acids ◽

Fractional Factorial Design ◽

Biological Activities ◽

Lactobacillus Rhamnosus ◽

Fractional Factorial ◽

Practical Application ◽

Steepest Ascent ◽

Freeze Dried ◽

Viable Bacteria

Abstract Currently research of lactic acid bacteria focus primarily on the functional probiotics, which are major beneficial biota in the gastrointestinal tract, have been industrial manufactured. Probiotics confer health benefits on the host need adequate amounts. However, the absence of data makes it difficult to ensure the maintenance biological activities and population of probiotic. In this research, a fractional factorial design and steepest ascent experiment were used to analyze the influence of lyoprotectant as carbohydrates, prebiotics and amino acids on the survival of the probiotic Lactobacillus rhamnosus. The results indicated a maximum survival rate and population of viable bacteria of L. rhamnosus to be 55.84 % and 1.60 ×1011 CFU/g after freeze-dried by using a combination of 10 g/100mL Sucrose, 2.5 g/100mL Isomaltooligosaccharide, 12 g/100mL Hydroxyproline. To a large extent, the survival and viability were dependent on the cryoprotectant used and make probiotics more attractive from a practical application in industrial viewpoint.

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

E-Journal of Chemistry ◽

10.1155/2010/470785 ◽

2010 ◽

Vol 7 (3) ◽

pp. 807-812 ◽

Cited By ~ 2

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.

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