Refinement of AOAC Official MethodSM 2005.06 Liquid Chromatography-Fluorescence Detection Method to Improve Performance Characteristics for the Determination of Paralytic Shellfish Toxins in King and Queen Scallops

2012 ◽  
Vol 95 (1) ◽  
pp. 129-142 ◽  
Author(s):  
Andrew D Turner ◽  
Robert G Hatfield
Keyword(s):  
Fluorescence Detection ◽  
Periodate Oxidation ◽  
Performance Characteristics ◽  
Official Method ◽  
Refined Method ◽  
Paralytic Shellfish ◽  
Aoac Official ◽  
Psp Toxins ◽  
Aoac Official Method

Abstract AOAC Official MethodSM 2005.06 LC-fluorescence detection (FLD) method is an official alternative to the mouse bioassay for the determination of paralytic shellfish poisoning (PSP) toxins in bivalve shellfish. To validate the method for species of relevance to the UK official control monitoring program, the method performance characteristics were tested for whole king and queen scallops. Validation showed that, while the performance was generally acceptable for the quantitation of non-N-hydroxylated toxins, poor toxin recovery and sensitivity was evident for the analysis of N-hydroxylated toxins following periodate oxidation. These effects occurred in a range of scallop samples with variable temporal and spatial sources. The effects were also noted in other laboratories following a small interlaboratory study. As a result, the method was refined to improve the recovery and sensitivity of analysis following the periodate oxidation step in the PSP method for scallops. Performance improved through alterations to the preparation of the periodate oxidant, use of higher volumes for C18 cleanup, and injection volumes in combination with the use of a king scallop matrix modifier for oxidation of N-hydroxylated toxin calibration standards. A single-laboratory validation of the refined method showed that the selectivity, linearity, sensitivity, recovery, and precision were acceptable and similar to values reported previously for AOAC Official Method 2005.06 in other bivalve species. Results showed the method to be rugged for all parameters investigated, including small changes to the composition of the new periodate reagent utilized in the refined method. The refined scallops LC method was subsequently compared with the European reference method. PSP-positive scallops showed an excellent agreement between the methods for queen and Atlantic scallops, with a small level of positive bias in the LC results for whole king scallops. These differences were related solely to the use of the highest toxicity equivalence factors for toxin epimeric pairs, with gonyautoxin (GTX)1,4 and GTX2,3 in particular present at high concentrations in the king scallops. Overall, the refined LC-FLD method improved the performance characteristics of AOAC Official Method 2005.06 for the determination of PSP toxins in whole king and queen scallops, and showed a good overall agreement between the official methodologies. It is, therefore, recommended as a more appropriate option for the routine monitoring of PSP toxins in these species.

Interlaboratory Comparison of Two AOAC Liquid Chromatographic Fluorescence Detection Methods for Paralytic Shellfish Toxin Analysis through Characterization of an Oyster Reference Material

2014 ◽  
Vol 97 (2) ◽  
pp. 380-390 ◽  
Author(s):  
Andrew D Turner ◽  
Adam M Lewis ◽  
Wade A Rourke ◽  
Wendy A Higman ◽  
Z Amzil ◽  
...  
Keyword(s):  
Reference Material ◽  
Fluorescence Detection ◽  
Official Method ◽  
Shellfish Poisoning ◽  
Paralytic Shellfish Toxin ◽  
Paralytic Shellfish ◽  
Shellfish Toxin ◽  
Aoac Official ◽  
Interlaboratory Reproducibility ◽  
Aoac Official Method

Abstract An interlaboratory ring trial was designed and conducted by the Centre for Environment, Fisheries, and Aquaculture Science to investigate a range of issues affecting the analysis of a candidate Pacific oyster paralytic shellfish toxin reference material. A total of 21 laboratories participated in the study and supplied results using one or more of three instrumental methods, specifically precolumn oxidation (Pre-COX) LC with fluorescence detection (FLD; AOAC Official Method 2005.06), postcolumn oxidation (PCOX) LC-FLD (AOAC Official Method 2011.02), and hydrophilic interaction LC/MS/MS. Each participant analyzed nine replicate samples of the oyster tissue in three separate batches of three samples over a period of time longer than 1 week. Results were reported in a standardized format, reporting both individual toxin concentrations andtotal sample toxicity. Data were assessed to determine the equivalency of the two AOAC LC methods and the LC/MS/MS method as well as an assessment of intrabatch and interbatch repeatability and interlaboratory reproducibility of each method. Differences among the results reported using the three methods were shown to be statistically significant, although visualcomparisons showed an overlap between results generated by the majority of tests, the exception being the Pre-COX quantitation of N-hydroxylated toxins in post ion-exchange fractions. Intralaboratory repeatability and interlaboratory reproducibility were acceptable for most of the results, withthe exception of results generated from fractions. The results provided good evidence for the acceptableperformance of the PCOX method for the quantitation of C toxins. Overall the study showed the usefulnessof interlaboratory analysis for the characterizationof paralytic shellfish poisoning matrix reference materials, highlighting some issues that may need to be addressed with further method assessment at individual participant laboratories.

Adaptation of the AOAC Fluorine Method for Determining Fluoride in Fish Protein Concentrate

1970 ◽  
Vol 53 (1) ◽  
pp. 3-6
Author(s):  
R. Bruce Klemm ◽  
Mary E. Ambrose Klemm
Keyword(s):  
Steam Distillation ◽  
Silica Sand ◽  
Official Method ◽  
Protein Concentrate ◽  
Fish Protein ◽  
Direct Titration ◽  
Modified Method ◽  
Aoac Official ◽  
Aoac Official Method

Abstract The AOAC official method, 24.029–24.035, for the determination of fluorine in foods was modified slightly to o btain quantitative recoveries of fluorine from samples of fish protein concentrate (FPC). The most important alterations include the use of steam distillation, the addition of finely ground silica sand in the distillation, a decrease in the distillation temperature, and the utilization of direct titration. Recoveries of fluoride added to FPC before ashing, using this modified method, averaged 96.0 ± 3.0%. Our results are in agreement with those of several other analysts who used a variety of methods.

Assessment of a Semiquantitative Liquid Chromatography- Fluorescence Detection Method for the Determination of Paralytic Shellfish Poisoning Toxin Levels in Bivalve Molluscs from Great Britain

2014 ◽  
Vol 97 (2) ◽  
pp. 492-497 ◽  
Author(s):  
Andrew D Turner ◽  
Monika Dhanji-Rapkova ◽  
Clothilde Baker ◽  
Myriam Algoet
Keyword(s):  
Great Britain ◽  
Fluorescence Detection ◽  
Detection Method ◽  
Reference Method ◽  
Paralytic Shellfish Poisoning ◽  
Official Method ◽  
Shellfish Poisoning ◽  
Bivalve Molluscs ◽  
Paralytic Shellfish

Abstract AOAC Official Method 2005.06 precolumn oxidation LC-fluorescence detection method has been used for many years for the detection and quantitation of paralytic shellfish poisoning (PSP) toxins in bivalve molluscs. After extensive single- and multiple-laboratory validation, the method has been slowly gaining acceptance worldwide as a useful and practical tool for official control testing. In Great Britain, the method has become routine since 2008, with no requirement since then for reverting back to the bioassay reference method. Although the method has been refined to be semiautomated, faster, and more reproducible, the quantitation step can be complex and time-consuming. An alternative approach was developed to utilize the qualitative screening results for generatinga semiquantitative results assessment. Data obtained over 5 years enabled the comparison of semiquantitative and fully quantitative PSP results in over 15 000 shellfish samples comprising eight different species showed that the semiquantitative approach resulted in over-estimated paralytic shellfish toxin levels by an average factor close to two in comparison with the fully quantified levels. No temporal trends were observed in the data or relating to species type, with the exception of surf clams. The comparison suggested a semiquantitative threshold of 800 μg saxitoxin (STX) eq/kg should provide a safe limitfor the determination of samples to be forwarded to full quantitation. However, the decision was taken to halve this limit to include an additional safety factor of 2, resulting in the use of a semiquantitative threshold of 400 μg STX eq/kg. Implementation of the semiquantitative method into routine testing would result in a significant reduction in the numbers of samples requiring quantitation and have a positive impact on the overall turnaround of reported PSP results. The refined method would be appropriate for any monitoring laboratory faced with high throughput requirements.

scholarly journals Akumulasi dan Depurasi Toksin PSP (Paralytic Shellfish Poisoning) oleh Kerang Hijau (Accumulation and Depuration of PSP Toxin (Paralytic Shellfish Poisoning) by Green Mussels)

2014 ◽  
Vol 19 (1) ◽  
pp. 27
Author(s):  
Haryoto Kusnoputranto ◽  
Setyo S Moersidik ◽  
Djarot S Wisnubroto ◽  
Murdahayu Makmur
Keyword(s):  
Paralytic Shellfish Poisoning ◽  
Perna Viridis ◽  
Official Method ◽  
Shellfish Poisoning ◽  
Toxin Concentration ◽  
Green Mussel ◽  
Mussel Farming ◽  
Paralytic Shellfish ◽  
Aoac Official ◽  
Aoac Official Method

Ledakan mikroalga sering dilaporkan terjadi di Teluk Jakarta, dimana di lokasi tersebut juga terdapat kegiatan budidaya kerang hijau (Perna viridis). Terkait dengan hal tersebut maka dilakukan studi akumulasi dan depurasi toksin PSP (Paralytic Shellfish Poisoning) pada kerang hijau. Studi akumulasi dilakukan di bagan kerang hijau perairan Cilincing Jakarta Utara, dengan memisahkan kerang hijau yang berukuran sama dan ditempatkan kembali ke bagan. Sampling dilakukan setiap minggu selama 2 bulan dan diukur juga kelimpahan fitoplankton, pH, suhu dan salinitas perairan. Depurasi dilakukan di Unit Depurasi Kekerangan KKP Panimbang Banten, yang dilakukan selama 24 jam. Pencuplikan  sampel dilakukan setiap jam pada 4 jam pertama dan setiap 2 dan 3 jam pada waktu berikutnya. Penentuan konsentrasi toksin PSP dilakukan dengan menggunakan HPLC detektor fluoresensi. Prosedur preparasi, ekstraksi dan pengukuran konsentrasi toksin mengikuti Manual AOAC Official Method 2005.06 untuk toksin PSP dalam kekerangan. Akumulasi toksin PSP oleh kerang hijau di perairan Cilincing pada bulan Januari–Pebruari 2011 berkisar antara 4,11–11,96 µg STX eq. per 100 g dan tidak mempunyai korelasi dengan kelimpahan Dinoflagelata di perairan. Hal ini disebabkan uji akumulasi tidak dilakukan pada saat blooming mikroalga. Uji depurasi selama 24 jam mengeliminasi toksin PSP sebesar 60%, sehingga bisa diajukan sebagai sistem pemutus rantai toksin dari mikroalga ke manusia. Kata kunci: akumulasi, depurasi, PSP toksin, kerang hijau, Cilincing Microalgae blooms have been frequently reported in the Jakarta Bay, which is also the location of green mussel (Perna viridis) aquaculture. Accumulation and depuration of Paralytic Shellfish Poisoning (PSP) toxin in the green mussels were investigated in the field, where the toxin accumulation studies conducted in the mussel farming at Cilincing, North Jakarta. Accumulation test carried out by placing back the selected green mussel (equal size) into the mussel farming. Every week for 2 months, the green mussel were collected from mussel farming and transported to the laboratory. The fitoplankton abundance also was checked including pH, Suhue and salinitiy paramaters. Toxin depuration was conducted at Clams Sanitation Unit at Panimbang Banten. The depuration studies were conducted for 24 hours with sampling every hour in the first 4 hours and every 3 and 2 hours until the 24th hour. Preparation, extraction and toxin concentration measurements performed by following the Manual AOAC Official Method 2005.06 for PSP toxin in oyster. This research concluded that the accumulation of PSP toxin by green mussel, Perna viridis in the mussel farming at Cilincing, North Jakarta in ranged between 4,11–11,96 µg STX eq. per 100 g during January–February 2011. No correlation between PSP toxin concentration in the green mussel, Perna viridis with abundance of the PSP toxin sources phytoplankton, because the study wasnt done when microalgae blooming. The depuration processes was eliminate 60% the PSP toxins for 24 hours depuration processing. It can be proposes as a banded system the PSP toxin from algae to human being. Keywords: accumulation, depuration, PSP toxin, green mussel, Cilincing

Allyl Isothiocyanate in Mustard Seed

1970 ◽  
Vol 53 (1) ◽  
pp. 1-3 ◽  
Author(s):  
Donald L Andersen
Keyword(s):  
Allyl Isothiocyanate ◽  
Mustard Seed ◽  
Official Method ◽  
Average Recovery ◽  
Aoac Method ◽  
Aoac Official ◽  
Mustard Seeds ◽  
Column Preparation ◽  
Aoac Official Method

Abstract A new GLC method for the determination of allyl isothiocyanate in mustard seed was compared to a method of the Midwest Research Institute and to a combination of the AOAC official method and the proposed method. Twelve collaborators compared the AOAC method and the GLC method, using whole mustard seeds. Each collaborator assayed three seed portions by both methods. The range, standard deviation, and coefficient of variation are less for each seed portion by the proposed than by the official method. The average recovery value of allyl isothiocyanate in the prepared standard solutions is lower, using the proposed GLC procedure, but seed assay values are significantly and consistently higher for each seed portion when compared with the results for the AOAC method. Reports from the collaborators also indicate that the proposed method is rugged, as the GLC column preparation was subjected to many changes. It is recommended that the GLC method be adopted as official first action.

scholarly journals Comparison of Babcock and Ether Extraction Methods for Determination of Fat Content of Cream: Collaborative Study

1996 ◽  
Vol 79 (4) ◽  
pp. 907-916 ◽  
Author(s):  
Joanna M Lynch ◽  
David M Barbano ◽  
J Richard Fleming
Keyword(s):  
Extraction Method ◽  
Collaborative Study ◽  
Extraction Methods ◽  
Fat Content ◽  
Official Method ◽  
Ether Extraction ◽  
Aoac Official ◽  
The Difference ◽  
Aoac Official Method

Abstract A modified Mojonnier ether extraction method for determination of the fat content of cream was developed based on the method for milk (AOAC Official Method 989.05). The cream Babcock method (AOAC Official Method 920.111 B-C) was modified to harmonize with the milk Babcock method (AOAC Official Method 989.04) and to clarify procedural details. Using the AOAC collaborative study format, 10 laboratories tested 9 pairs of blind duplicate heat-treated cream samples with a fat range of 30-45% using both methods. The statistical performance (invalid and outlier data removed) was as follows: mean % fat = 37.932, sr = 0.125, sR = 0.151, RSDr = 0.330, RSDR = 0.398, r = 0.354, and R = 0.427 for the ether extraction method. For the Babcock method, mean % fat = 38.209, sr = 0.209, SR = 0.272, RSDr = 0.548, RSDR = 0.712, r = 0.592, and R = 0.769. Average test results for fat from the Babcock method were 0.277% (absolute fat) greater than for the Mojonnier ether extraction method. The difference between methods, as a percentage of the average fat content of the samples, was 0.73%. This agrees with differences observed between the 2 methods for milk when 10 to 17 laboratories tested 7 milk samples in blind duplicate at bimonthly intervals over a 4-year period (average difference 0.029% fat, 0.78% as a percentage of average fat content). The Mojonnier ether extraction and Babcock methods for fat in cream have been adopted by AOAC INTERNATIONAL. The new Babcock method replaced the AOAC Official Method 920.111 B-C.

scholarly journals Determination of Total Dietary Fiber in Selected Foods Containing Resistant Maltodextrin by a Simplified Enzymatic-Gravimetric Method and Liquid Chromatography: Interlaboratory Study in China

2008 ◽  
Vol 91 (3) ◽  
pp. 614-621 ◽  
Author(s):  
Boqiang Fu ◽  
Jing Wang ◽  
Jean Michel Roturier ◽  
Zhiyu Tang ◽  
Huan Li ◽  
...  
Keyword(s):  
Dietary Fiber ◽  
Interlaboratory Study ◽  
National Standard ◽  
Official Method ◽  
Total Dietary Fiber ◽  
Modified Method ◽  
Resistant Maltodextrin ◽  
Aoac Official ◽  
Aoac Official Method

Abstract An interlaboratory study was conducted in China to validate the modified AOAC Official Method 2001.03 for the determination of total dietary fiber (TDF) in foods containing resistant maltodextrin (RMD), which will be adopted as the National Standard Method of China. The kind of buffer solution, the volume of filtrate evaporation, the volume of eluent for desalting and residual solution after evaporation, etc. were modified, which had been proved to have acceptable accuracy and precision in the routine assay. TDF contents in 3 representative foods and 2 kinds of RMD ingredient (i.e., NUTRIOSE 06 and NUTRIOSE 10) were measured using the modified method in 6 eligible laboratories representing commercial, industrial, and governmental laboratories in China. The results of the interlaboratory study indicated that the intralaboratory repeatability, interlaboratory reproducibility, and precision of the modified method are adequate for reliable analysis of TDF in food containing RMD, as well as resistant dextrin. Compared to AOAC Official Method 2001.03, the modified method is time- and cost-saving.

scholarly journals Liquid Chromatographic Determination of Pyrantel Tartrate in Medicated Formulations

2003 ◽  
Vol 86 (5) ◽  
pp. 882-887
Author(s):  
Joyce A Konrardy ◽  
Mary A Burner ◽  
Tommy W Garner ◽  
Mark A Litchman ◽  
Gregory K Webster
Keyword(s):  
Chromatographic Determination ◽  
Official Method ◽  
Stability Indicating ◽  
Stability Indicating Method ◽  
Liquid Chromatographic Determination ◽  
Aoac Official ◽  
Liquid Chromatographic ◽  
Aoac Official Method ◽  
Pyrantel Tartrate

Abstract The validation of a novel liquid chromatographic (LC) method for the determination of pyrantel tartrate in feed is presented. The method provides a significant improvement over the efficiency and precision of AOAC Official Method 978.30. The method was shown to be accurate, precise, linear, and robust for medicated articles. Unlike the official method, the LC method was shown to be a superior stability-indicating method. After the method was validated by using laboratory blends, the effectiveness of the method was demonstrated with marketed product as well.

Determination of Formaldehyde in Maple Sirup: Interfering Substances

1972 ◽  
Vol 55 (1) ◽  
pp. 121-122
Author(s):  
J C Underwood
Keyword(s):  
Mass Spectrometry ◽  
Carbonyl Compounds ◽  
Official Method ◽  
Formaldehyde Determination ◽  
Aoac Official ◽  
Aoac Official Method

Abstract Three carbonyl compounds isolated from maple sirup by distillation as in the AOAC official method for formaldehyde have been identified by mass spectrometry as formaldehyde, acetone, and acetaldehyde. Acetone and acetaldehyde do not interfere with the formaldehyde determination if the procedure of the AOAC official method is followed; acetol and glyoxal also do not cause errors in the formaldehyde value. Tests run have shown the modified Nash method (31.184–31.189) adopted as official final action to be extremely specific for formaldehyde in maple sirup.

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