Simplified Spectrophotometric Curcumin Method for the Determination of Boron in Marine Shellfish

1975 ◽  
Vol 32 (6) ◽  
pp. 813-816 ◽  
Author(s):  
R. E. Drew
Keyword(s):  
Hydrogen Peroxide ◽  
Standard Deviation ◽  
Acetic Anhydride ◽  
Sulphuric Acid ◽  
Relative Standard Deviation ◽  
Tissue Sample ◽  
Total Error ◽  
Relative Standard ◽  
Wet Weight

The method involves a sulphuric acid–hydrogen peroxide digestion of the tissue sample at 100 C, dehydration of the digest with acetic anhydride, formation of the boron–curcumin complex (rosocyanin), followed by buffering of the solution and measurement of the absorbance at 545 nm. Data are presented to show that a mean relative standard deviation of approximately 5% and a mean total error of approximately 12% can be expected for shellfish in the concentration range of 1.0–10.0 μg B/g wet weight tissue (ppm).

Kinetic Spectrophotometric Determination of Selenium (IV) by its Catalytic Effect on the Oxidation of Acid Chrome Blue K by Hydrogen Peroxide

2012 ◽  
Vol 538-541 ◽  
pp. 2358-2363 ◽  
Author(s):  
Zhi Rong Zhou ◽  
Li Zhen Zhang
Keyword(s):  
Hydrogen Peroxide ◽  
Standard Deviation ◽  
Relative Standard Deviation ◽  
Limit Of Detection ◽  
Fixed Time ◽  
Relative Standard ◽  
Kinetic Spectrophotometric ◽  
Acid Chrome Blue K ◽  
Good Agreement

Based on the oxidation of acid chrome blue K (ACBK) by hydrogen peroxide in 0.002 mol/L sulfuric acid solution, while 1,10-phenanthroline (phen) acts as an activator, a simple kinetic spectrophotometric method was developed for the determination of trace amounts of Se(IV).The reaction was monitored spectrophotometrically by measuring the decrease in the absorbance of ACBK at 524 nm with a fixed-time method. The decrease in the absorbance of ACBK is proportional to the concentration of Se (IV) in the range 0.06–1.0 µg/L with a fixed time of 4–10 min from the initiation of the reaction. The limit of detection is 0.018 µg/L Se (IV). The influence of the factors such as acidity, concentration of reactants, reaction time, temperature and co-existing ions on the reaction is discussed. The optimum conditions of reaction are established and some kinetic parameters are determined. The apparent activation energy of catalytic reaction is 62.30 kJ/mol. The relative standard deviation for 11 replicate determination of 0.01 and 0.02 µg/25mL selenium (III) was calculated to be 2.3 % and 2.0 %, respectively. Combined with sulphydryl dextrane gel (SDG) separation and enriching, the method has been successfully applied to the determination of Se (IV) in foodstuff samples with the relative standard deviation of 1.1 %–3.7 % and the recovery of 99.0 %–104.0 %, the results are in good agreement with those provided by HG-AAS method.

Enzymatic Determination of Sulfite in Foods: NMKL Interlaboratory Study

1993 ◽  
Vol 76 (1) ◽  
pp. 53-58 ◽  
Author(s):  
Ulla Edberg ◽  
◽  
Maija-Liisa Anttonen ◽  
Karen Berg-Nilsen ◽  
Karin Blomberg ◽  
...  
Keyword(s):  
Hydrogen Peroxide ◽  
Standard Deviation ◽  
Relative Standard Deviation ◽  
Collaborative Study ◽  
Study Data ◽  
Relative Standard ◽  
Full Study ◽  
Potato Flakes ◽  
Reduced Nicotinamide Adenine Dinucleotide

Abstract An enzymatic method for the determination of sulfite in foods was collaboratively studied in Nordic industry and government laboratories. The sulfite in liquid foods or extracts of solid foods is analyzed according to the following principle: Sulfite ions are oxidized to sulfate ions by oxygen in the presence of sulfite oxidase, thereby forming hydrogen peroxide. Hydrogen peroxide is transformed to water by reduced nicotinamide adenine dinucleotide (NADH) in the presence of NADH peroxidase. In this reaction, NAD+ is formed (and NADH is consumed) in amounts proportional to the sulfite concentration. Consumption of NADH can be measured spectro photo metrically at 340 nm. The method was collaboratively tested in 2 separate studies with high and low levels of sulfite tested. Results of both studies are reported here. The study samples consisted of potato flakes, wine, juice, and dried apples containing between 0 and about 960 mg SCVkg. Eleven laboratories participated in the full study and analyzed 12 samples. Six laboratories analyzed 8 samples in the complementary study. Before statistical evaluation of the collaborative study data, results were adjusted for the time-dependent decrease of sulfite in the case of materials with high sulfite content (dried apples and wine). For 2 blind duplicate samples of wine containing 75 mg S02/kg, the relative standard deviation for repeatability (RSDR, within-laboratory variation) was 3.9%. Relative standard deviation for reproducibility (RSDR, between-laboratory variation) was 7.6%. For 2 samples of dried apples containing 800 and 960 mg S02/kg, an RSDr value of 13.3% and an RSDR value of 13.9% were calculated. The corresponding parameters for 2 juice samples containing about 270 mg S02/kg were 4.8 and 10.4% for repeatability and reproducibility, respectively.

An Automated Procedure for the Determination of Ammonia in Tobacco

1972 ◽  
Vol 6 (4) ◽  
Author(s):  
P.F. Collins ◽  
W.W. Lawrence ◽  
J.F. Williams
Keyword(s):  
Standard Deviation ◽  
Relative Standard Deviation ◽  
Distillation Method ◽  
Relative Standard ◽  
Tobacco Sample ◽  
Automated Determination

AbstractA procedure for the automated determination of ammonia in tobacco has been developed. Ammonia is extracted from the ground tobacco sample with water and is determined with a Technicon Auto Analyser system which employs separation of the ammonia through volatilization followed by colourimetry using the phenate-hypochlorite reaction. The procedure has been applied to a variety of tobaccos containing from 0.02 to 0.5 % ammonia with an overall relative standard deviation of 2 %. The accuracy of the procedure as judged by recovery tests and by comparison to a manual distillation method is considered adequate

scholarly journals Indirect and Direct Determination of the Casein Content of Milk by Kjeldahl Nitrogen Analysis: Collaborative Study

1998 ◽  
Vol 81 (4) ◽  
pp. 763-774 ◽  
Author(s):  
Joanna M Lynch ◽  
David M Barbano ◽  
J Richard Fleming
Keyword(s):  
Standard Deviation ◽  
Nitrogen Content ◽  
Relative Standard Deviation ◽  
Collaborative Study ◽  
Direct Determination ◽  
Raw Milk ◽  
Method Performance ◽  
Relative Standard ◽  
Milk Casein

Abstract The classic method for determination of milk casein is based on precipitation of casein at pH 4.6. Precipitated milk casein is removed by filtration and the nitrogen content of either the precipitate (direct casein method) or filtrate (noncasein nitrogen; NCN) is determined by Kjeldahl analysis. For the indirect casein method, milk total nitrogen (TN; Method 991.20) is also determined and casein is calculated as TN minus NCN. Ten laboratories tested 9 pairs of blind duplicate raw milk materials with a casein range of 2.42- 3.05℅ by both the direct and indirect casein methods. Statistical performance expressed in protein equivalents (nitrogen ⨯ 6.38) with invalid and outlier data removed was as follows: NCN method (wt%), mean = 0.762, sr = 0.010, SR = 0.016, repeatability relative standard deviation (RSDr) = 1.287℅, reproducibility relative standard deviation (RSDR) = 2.146%; indirect casein method (wt℅), mean = 2.585, repeatability = 0.015, reproducibility = 0.022, RSDr = 0.560℅, RSDR = 0.841; direct casein method (wt℅), mean = 2.575, sr = 0.015, sR = 0.025, RSDr = 0.597℅, RSDR = 0.988℅. Method performance was acceptable and comparable to similar Kjeldahl methods for determining nitrogen content of milk (Methods 991.20, 991.21,991.22, 991.23). The direct casein, indirect casein, and noncasein nitrogen methods have been adopted by AOAC INTERNATIONAL.

Determination of Nitrate in Water by HPLC

2013 ◽  
Vol 448-453 ◽  
pp. 406-408
Author(s):  
Jing Liu ◽  
Xiao Na Ji ◽  
Qing Kai Ren ◽  
Sheng Shu Ai ◽  
Li Jun Wan ◽  
...  
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Standard Deviation ◽  
Relative Standard Deviation ◽  
Recovery Rate ◽  
High Performance ◽  
Separation Efficiency ◽  
Fast Analysis ◽  
Relative Standard

We established a method fordetermination of nitrate in water by High Performance Liquid Chromatography(HPLC). The sample was analysed by HPLC-ADA and was quantitated by externalstandard method after being simply processed. This methd has the advantages ofhigh separation efficiency and fast analysis. The experiment result showed thatthe linearly dependent coefficient was0.994, the recovery rate was between 98.7%～105.7%,the relative standard deviation（RSD）wasless than 2.1 %, and the lowest detectable limit is 0.01ng (S/N=1.6).

scholarly journals Determination of 1,3-Dichloropropanol in Soy Sauce and Related Products by Headspace Gas Chromatography with Mass Spectrometric Detection: Interlaboratory Study

2005 ◽  
Vol 88 (5) ◽  
pp. 1404-1412 ◽  
Author(s):  
Sarah Hasnip ◽  
Colin Crews ◽  
Nicholas Potter ◽  
Paul Brereton ◽  
Henri Diserens ◽  
...  
Keyword(s):  
Gas Chromatography ◽  
Standard Deviation ◽  
Relative Standard Deviation ◽  
Internal Standard ◽  
Mass Spectrometric ◽  
Soy Sauce ◽  
Headspace Gas Chromatography ◽  
Relative Standard ◽  
Headspace Gas

Abstract An interlaboratory study was performed to evaluate the effectiveness of a headspace gas chromatography (GC) method for the determination of 1,3-dichloro-propan-2-ol (1,3-DCP) in soy sauce and related products at levels above 5 ng/g. The test portion is mixed with an internal standard (d5-1,3-DCP) and ammonium sulfate in a sealed headspace vial. After achieving equilibrium, the headspace is sampled either by gas-tight syringe or solid-phase microextraction (SPME) and analyzed by GC with mass spectrometric detection. 1,3-DCP is detected in the selected-ion mode (monitoring m/z 79 and 81 for 1,3-DCP and m/z 82 for the deuterated internal standard) and quantified by measurement against standards. Test materials comprising soy, dark soy, mushroom soy, and teriyaki sauces, both spiked and naturally contaminated, were sent to 9 laboratories in Europe, Japan, and the United States; of these, 5 used SPME and 4 used syringe headspace analysis. Test portions were spiked at 5.0, 10.0, 20.0, 100.0, and 500.0 ng/g. The average recovery for spiked blank samples was 108% (ranging from 96–130%). Based on results for spiked samples (blind pairs at 5, 10, 20, 100, and 500 ng/g) as well as a naturally contaminated sample (split-level pair at 27 and 29 ng/g), the relative standard deviation for repeatability (RSDr) ranged from 2.9–23.2%. The relative standard deviation for reproducibility (RSDR) ranged from 20.9–35.3%, and HorRat values of between 1.0 and 1.6 were obtained.

scholarly journals Development and validation of spectrophotometric method for phenylephrine hydrochloride estimation in nasal drops formulations

2008 ◽  
Vol 27 (2) ◽  
pp. 149 ◽  
Author(s):  
Ivana Savić ◽  
Goran Nikolić ◽  
Vladimir Banković
Keyword(s):  
Standard Deviation ◽  
Sodium Hydroxide ◽  
Relative Standard Deviation ◽  
Spectrophotometric Method ◽  
Molar Absorptivity ◽  
Dosage Forms ◽  
Phenylephrine Hydrochloride ◽  
Relative Standard ◽  
Development And Validation

Simple, accurate and reproducible UV-spectrophotometric method was developed and validated for the estimation of phenylephrine hydrochloride in pharmaceutical nasal drops formulations. Phenylephrine hydrochloride was estimated at 291 nm in 1 mol⋅dm-3 sodium hydroxide (pH 13.5). Beer’s law was obeyed in the concentration range of 10–100 μg⋅cm−3 (r2 = 0.9990) in the sodium hydroxide medium. The apparent molar absorptivity was found to be 1.63×103 dm3⋅mol−1⋅cm−1. The method was tested and validated for various parameters according to the ICH (International Conference on Harmonization) guidelines. The detection and quantitation limits were found to be 0.892 and 2.969 μg⋅cm−3, respectively. The proposed method was successfully applied for the determination of phenylephrine hydrochloride in pharmaceutical nasal drops formulations. The results demonstrated that the procedure is accurate, precise and reproducible (relative standard deviation < 1 %), while being simple, cheap and less time consuming, and hence can be suitably applied for the estimation of phenylephrine hydrochloride in different dosage forms.

scholarly journals Badanie stabilności barwnych znaczników fluorescencyjnych w silnie zasiarczonych wodach złożowych

Nafta-Gaz ◽  
2021 ◽  
Vol 77 (2) ◽  
pp. 82-91
Author(s):  
Katarzyna Wojtowicz ◽  
Keyword(s):  
Standard Deviation ◽  
Relative Standard Deviation ◽  
Rhodamine B ◽  
Water Reservoir ◽  
Distilled Water ◽  
Test Results ◽  
Fluorescent Tracers ◽  
Reservoir Water ◽  
Relative Standard

The article presents the issues related to the determination of colored fluorescent tracers such as fluorescein, eosin yellowish, rhodamine B and uranine in reservoir waters by spectrophotometric method. For this purpose, the influence of the pH of the solution on the absorption spectra of the tested tracers was checked. Test results show that fluorescein, rhodamine B and uranine are sensitive to changes in the buffer pH, therefore it is advisable to use stable tracer solutions as well as to control and possibly correct pH in further tests. As part of the study, calibration curves of fluorescein, eosin yellowish, rhodamine B and uranine in distilled water, reservoir water A4 and highly sulfated reservoir waters A5 and A6 were plotted and the analytical methods were validated. Analytical validation included determination of linearity, standard deviation and relative standard deviation of the tested tracers solutions. High values of the regression parameters (0.9927–0.9998) of the analyzed tracers prove a good linear fit, while low values of standard deviation and relative standard deviation prove its repeatability and precision. Particular attention was paid to testing the stability of colored fluorescent tracers in highly sulfated reservoir waters. For this purpose, solutions of the tested tracers were prepared at concentrations of 10 mg/dm3 in distilled water, A4 reservoir water and highly sulfated A5 and A6 reservoir waters. Measurements of the tested tracers in the prepared solutions were performed every 2 days over the period of 1 month. The test results show that fluorescein, eosin yellowish, rhodamine B and uranine solutions are stable in the distilled water and A4 reservoir water, while they degrade in the A5 and A6 reservoir waters. Fluorescein and uranine turned out to be the most sensitive, as they degraded completely in the A6 reservoir water after 20 (fluorescein) and 22 (uranine) days. Yellowish eosin and rhodamine B turned out to be slightly more stable in highly sulfated reservoir waters, as they degraded completely in the A6 reservoir water after 24 days.

scholarly journals Interlaboratory Evaluation of Two Enzyme-Linked Immunosorbent Assay Kits for the Determination of Crustacean Protein in Processed Foods

2008 ◽  
Vol 91 (1) ◽  
pp. 123-129 ◽  
Author(s):  
Shinobu Sakai ◽  
Rieko Matsuda ◽  
Reiko Adachi ◽  
Hiroshi Akiyama ◽  
Tamio Maitani ◽  
...  
Keyword(s):  
Standard Deviation ◽  
Relative Standard Deviation ◽  
Immunosorbent Assay ◽  
Soluble Protein ◽  
Enzyme Linked Immunosorbent Assay ◽  
Processed Foods ◽  
Relative Standard ◽  
High Level

Abstract The labeling of foods containing material derived from crustaceans such as shrimp and crab is to become mandatory in Japan because of increases in the number of allergy patients. To ensure proper labeling, 2 novel sandwich enzyme-linked immunosorbent assay (ELISA) kits for the determination of crustacean protein in processed foods, the N kit (Nissui Pharmaceutical Co., Ltd, Ibaraki, Japan) and the M kit (Maruha Nichiro Holdings, Inc., Ibaraki, Japan), have been developed. Five types of model processed foods containing 10 and/or 11.9 g/g crustacean soluble protein were prepared for interlaboratory evaluation of the performance of these kits. The N kit displayed a relatively high level of reproducibility relative standard deviation (interlaboratory precision; 4.08.4 RSDR) and sufficient recovery (6586) for all the model processed foods. The M kit displayed sufficient reproducibility (17.620.5 RSDR) and a reasonably high level of recovery (82103). The repeatability relative standard deviation (RSDr) values regarding the detection of crustacean proteins in the 5 model foods were mostly &lt;5.1 RSDr for the N kit and 9.9 RSDr for the M kit. In conclusion, the results of this interlaboratory evaluation suggest that both these ELISA kits would be very useful for detecting crustacean protein in processed foods.

scholarly journals Liquid Chromatographic Determination of Ampicillin Residues in Porcine Muscle Tissue by a Multipenicillin Analytical Method: European Collaborative Study

2002 ◽  
Vol 85 (4) ◽  
pp. 889-900 ◽  
Author(s):  
Eric Verdon ◽  
Pierric Couëdor ◽  
Pierre Maris ◽  
Michel Laurentie ◽  
P Batjoens ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Standard Deviation ◽  
Relative Standard Deviation ◽  
Muscle Tissue ◽  
Phosphate Buffer ◽  
Collaborative Study ◽  
Porcine Muscle ◽  
Relative Standard ◽  
Liquid Chromatographic

Abstract A collaborative study involving 14 laboratories was conducted to determine residues of ampicillin in porcine muscle tissue by using a liquid chromatographic method developed for multipenicillin analysis that can quantitate 8 penicillin compounds (benzylpenicillin, phenoxymethylpenicillin, ampicillin, amoxicillin, nafcillin, oxacillin, cloxacillin, and dicloxacillin) at trace levels in muscle tissue. This method involves extraction of the penicillins with phosphate buffer, pH 9, followed cleanup and concentration on a C18 solid-phase extraction column and reaction with benzoic anhydride at 50°C and with 1,2,4-triazole and mercury(II) chloride solution, pH 9.0, at 65°C. The derivatized compounds are eluted isocratically on a C8 column with a mobile phase of acetonitrile and phosphate buffer (pH 6; 0.1M) containing sodium thiosulfate and the ion-pair reagent tetrabutylammonium hydrogen sulfate. The penicillins are detected by UV absorption at 325 nm. The limit of detection and the limit of determination (quantitation) of the method were calculated to be approximately 3–5 and 25 μg/kg, respectively, in accordance with the criteria of European Union (EU) Decision No. 93/256/EEC. In this first interlaboratory study, collaborators were instructed to monitor 4 different penicillin compounds (benzylpenicillin, phenoxymethylpenicillin, ampicillin, and amoxicillin) by analyzing 8 blind samples of muscle tissue in triplicate. These samples were prepared from 2 materials containing different concentrations of incurred ampicillin (63.5 μg/kg for material No. 1 and 358.1 μg/kg for material No. 2) and 1 blank material. The repeatability relative standard deviation and the reproducibility relative standard deviation were 10.2 and 17.4%, respectively, for material No. 1 and 7.0 and 16.0%, respectively, for material No. 2. These results demonstrate that the method is suitable for the determination of ampicillin residues in muscle tissue at the EU maximum residue limit (50 μg/kg) and above. However, the identification of positives by this procedure may need additional confirmation by techniques with greater specificity, such as liquid chromatography combined with mass spectrometry, or tandem mass spectrometry. Investigations regarding the basis of interlaboratory testing studies will further demonstrate the suitability of multiresidue methodology for detecting and quantitating other compounds in the family of penicillin antibiotics.

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