Collaborative Study of Accuracy and Precision of Rapid Determination of Fat in Meat and Meat Products by Foss-Let Method

1977 ◽  
Vol 60 (4) ◽  
pp. 853-858 ◽  
Author(s):  
Julio D Pettinati ◽  
Clifton E Swift

Abstract Collaborators in 12 meat and food industry laboratories performed 4 fat determinations each on 7 samples of meat and meat products by the rapid (7–10 min) Foss-Let method and compared the results with those obtained by AOAC method 24.005(a) or 24.005(b). From the overall mean of results on all samples, determinations by the Foss-Let method averaged 0.11% fat higher than by the AOAC method. This difference was not significant by the t-test (P = 0.05), which indicated agreement between the compared methods in determining fat content. Precision of the Foss-Let method was equivalent to and generally slightly better than that of the AOAC method. Standard deviations with the Foss-Let method were 0.2 % fat for between-duplicates and for within-laboratory repeatability; 0.4% fat for between-laboratories, including variation due to laboratory-sample interaction; and 0.5% fat for reproducibility between analysts in different laboratories. The Foss-Let method has been adopted as official first action.

1977 ◽  
Vol 60 (3) ◽  
pp. 600-608
Author(s):  
Julio D Pettinati ◽  
Clifton E Swift

Abstract A collaborative study of determination of fat by AOAC method 24.005(a) or (b) was conducted to gain more knowledge regarding its characteristics of precision. Twelve analysts in meat and food industry laboratories each performed 4 determinations on 7 samples containing 3.4–48% fat. The following characteristics of precision of the method were established: Variation between duplicate determinations was 0.3% fat; within-laboratory repeatability on separate days was 0.3% fat for samples containing up to 27% fat and 0.7% for samples containing 48% fat; variation among laboratories, including variation due to laboratory-sample interaction, was 0.4% fat; and reproducibility, which includes variations of determinations on a sample by different analysts using different sets of equipment in different laboratories, was 0.6% fat. This information is especially useful for comparative evaluations of alternative methods of fat determination.


1984 ◽  
Vol 67 (3) ◽  
pp. 637-640 ◽  
Author(s):  
David O Biltcliffe ◽  
Dick H Kleyn ◽  
J Richard Trout ◽  
◽  
D Azzara ◽  
...  

Abstract Collaborators in 8 dairy and food industry laboratories performed one lactose determination on each of 8 unknown samples of milk, lowfat milk, or skim milk, as 3 pairs of blind duplicates. Two known samples were provided to gain experience prior to analysis of the unknown samples. All of the above samples were also analyzed for lactose content by the official AOAC gravimetric method (16.507) by a commercial laboratory. From the overall mean of results on all samples, determinations by the enzymatic method averaged 0.49% lower than by the AOAC method. This difference was significant by the t-test (P = 0.05), which indicated a lack of agreement between the compared methods in determining lactose content. Standard deviations were similar for the 3 sets of blind duplicates which ranged between 3.67 and 4.55% lactose content. F-values revealed that variations between means obtained by laboratories differed significantly as compared with variations within laboratory means. The method has been adopted official first action.


1981 ◽  
Vol 64 (3) ◽  
pp. 704-708
Author(s):  
Luis F Corominas ◽  
Víctor M Boy ◽  
Pedro Rojas

Abstract The AOAC official first action method, 2.147-2.150, for flame emission spectrophotometry (FES) determination of sodium in fertilizers was compared with the atomic absorption spectrophotometric (AAS) method and the sodium selective electrode (SSE) method. Ammonium oxalate, which was previously compared with water, H2SO4, HC1, and HNO3, was used to extract the sample for all 3 methods. Three synthetic NPK samples, 3 commercial samples (urea, normal superphosphate, and neutrophos), 1 phosphate rock, and 2 Magruder check samples were used for the study. Statistically significant differences were obtained in averages for most of the samples, but few differences were found in standard deviations. The AAS method showed the best accuracy and precision. Accuracy of the AOAC method is acceptable. The SSE method showed the highest deviations from the theoretical values. A collaborative study is recommended to compare the AOAC with the AAS method.


1975 ◽  
Vol 58 (6) ◽  
pp. 1182-1187
Author(s):  
Julio D Pettinati ◽  
Clifton E Swift

Abstract The commercially available Foss-let fat analyzer was evaluated for the determination of fat in meat and meat products by comparison with AOAC method 24.005(a). With the Foss-let procedure, mechanical and instrumental equipment is used to determine fat in 7–10 min. A sample is extracted with tetrachloroethylene in a mechanical orbital shaker for 2 min and the specific gravity of the extract is measured in a magnetic float cell controlled by a digital potentiometer. During extraction, anhydrous calcium sulfate absorbs moisture droplets originating from the sample. The variations of comparative determinations on 67 meat samples containing 1.1–95.4% fat and 17 frankfurter samples containing 17.3–37.3% fat were analyzed statistically by grouping the data according to meat type (beef or pork) or frankfurters and into 6 ranges of fat content, and by treating the entire set of data. Error analysis of the differences and standard deviation of each grouping of paired determinations by the Fosslet and AOAC methods indicated that meat type and fat content >7.5% were not significant (P = 0.05) sources of variation as determined by t-tests on the statistics from the blocks of data. Determinations on samples containing ≤7.5% fat were consistently low and an additive correction of 0.25% was indicated. From the overall results, the accuracy and precision of the method were characterized as follows: the mean Foss-let method determination was high by 0.08% fat relative to that by the AOAC method; repeatability of ± 0.31% fat between duplicate determinations compared favorably with ±0.38% obtained with the AOAC method; and precision between paired determinations by the 2 methods was ±0.44%. Both a t-test for significance (P = 0.05) and the linear regression of the 84 comparative determinations indicated that the Foss-let method was equivalent to the AOAC method for determining fat.


1992 ◽  
Vol 75 (6) ◽  
pp. 1016-1022 ◽  
Author(s):  
Kurt Kolar

Abstract Fourteen laboratories participated in a collaborative study of gravimetric methods for determination of moisture and ash in meat and meat products. The determination of moisture by drying without sand at 102-105C for 16-18 h and to constant weight was compared with the official NMKL method using drying with sand to constant weight. The incineration was performed at 550°C. The method was tested on 16 blind duplicate samples of fresh meat and meat products ranging in moisture content from 44.1 to 74.8 g/100 g, and in ash content from 1.0 to 5.4 g/100 g. Drying without sand for 16-18 h and to constant weight gave no significant difference. Therefore, the labor-intensive drying to constant weight is not necessary to obtain reliable results. In comparison with the official NMKL method based on drying with sand, the mean values, repeatability, and reproducibility of the drying method without sand for 16-18 h agree very well. Therefore, there is no reason to retain the more complicated and labor-intensive sand drying method. The conditions of the proposed method differ only slightly from the conditions used in the official AOAC method, 950.46 B(a). The collaborative results for the determination of both moisture and ash gave estimates for precision according to the HORRAT values


1993 ◽  
Vol 76 (4) ◽  
pp. 902-906 ◽  
Author(s):  
Sami M Al-Hasani ◽  
Jan Hlavac ◽  
Mark W Carpenter

Abstract A rapid method has been developed for cholesterol determination in single and multicomponent foods. The method involves alcoholic KOH saponification of the samples, extraction of the nonsaponif iable fraction with hexane, and injection of concentrated extract into the gas chromatograph without derivatizations. It has been applied to a wide variety of frozen and refrigerated foods. More than 300 samples were analyzed with a coefficient of variation (CV) ranging from 0.5 to 8.6%. The average recoveries of cholesterol from spiked oil and tomato vegetable soup samples were 100 ±1.5% and 99.7 ±1.6% and the CVs were 1.5 and 1.6%, respectively. This method reduces labor by >70%, eliminates dangerous chemicals, and minimizes solvent use, compared to the AOAC method and other methods cited in the manuscript. The method was used successfully on a wide variety of multicomponent foods. We recommend this method for collaborative study under the AOAC guidelines for method approval.


1974 ◽  
Vol 57 (4) ◽  
pp. 838-840
Author(s):  
Walter M Gantenbein ◽  
Jon L Schermerhorn ◽  
Elmer George

Abstract An automated method for nitrogen in meat products was studied collaboratively. Samples were solubilized in sulfuric acid (1 + 1) , cooled to room temperature, and presented to an automated system. Digestion, dilution, and colorimetric measurement of the nitrogen were performed automatically. Samples were also analyzed by the official final action AOAC method, 24.010. Eight collaborators representing 6 laboratories participated in the study. Each participant analyzed 9 different samples in duplicate. Results of the study were satisfactory with an average range of 0.5% protein, average standard deviation of ±0.21%, and average coefficient of variation of 1.20%. The method was found to be as accurate as 24.010 and applicable to meat and meat products containing 0.8–4.0% nitrogen (5.0–25% protein). It has been adopted as official first action.


1973 ◽  
Vol 56 (6) ◽  
pp. 1313-1318
Author(s):  
Julio D Pettinati ◽  
Edward H Cohen

Abstract A method utilizing azeotropic distillation for determining moisture and fat in the same sample of ground beef, frankfurters, or pork sausage was collaboratively studied. The apparent moisture content of these products, determined by measuring the volume of condensate after 30 min distillation with cumene, m-xylene, or ethylbenzene, was 1 % lower than that determined by method 24.003(a). The fat content was determined by weighing the residue from an aliquot of the extract taken after 30 min (ground beef and frankfurters) or 45 min (pork) distillation. The fat content of ground beef and frankfurters, determined by using all 3 solvents, agreed with results obtained by method 24.005(a); results for pork samples were about 1% low. Significant positive correlation (r = 0.99) was obtained for both moisture and fat data with results from the AOAC methods. Statistical evaluation of the collaborative results for the 3 meat products, using the 3 solvents, led to expected standard deviations, se, of ±0.94% moisture and ±1.03% fat. Azeotropic distillation with cumene, m-xylene, or ethylbenzene is useful as a rapid screening procedure for determining moisture and fat in meats prior to processing or in finished products where rapid analysis is more important than maximum accuracy and precision.


Molecules ◽  
2021 ◽  
Vol 26 (14) ◽  
pp. 4357
Author(s):  
Waritda Pookmanee ◽  
Siriwan Thongthip ◽  
Jeeranut Tankanitlert ◽  
Mathirut Mungthin ◽  
Chonlaphat Sukasem ◽  
...  

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.


Sign in / Sign up

Export Citation Format

Share Document