Contains Confidential Business Information Subject To Protective Order
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`UNITED STATES INTERNATIONAL TRADE COMMISSION
`WASHINGTON, D.C. 20436
`
`Before The Honorable Theodore R. Essex
`
`Administrative Law Judge
`
`In the Matter of
`
`CERTAIN OMEGA-3 EXTRACTS FROM
`MARINE OR AQUATIC BIOMASS AND
`PRODUCTS CONTAINING THE SAME
`
`Investigation No. 337-TA-877
`
`REBUTTAL WITNESS STATEMENT OF DR. JACEK JACZYNSKI
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`158. Q: What is the significance, if any, of Mr. Haugsgjerd’s added steps of
`flushing oil fractions with nitrogen gas and freezing them at -20°C before
`heating?
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`A: These steps would have suppressed the heat-induced hydrolysis that would
`occur during heating of the samples to 125°C, as required by Beaudoin I, or to 60-
`70°C, as required by Beaudoin II, which was performed later by Dr. Gundersen.
`
`160. Q: Did Dr. Gundersen properly heat the samples according to the Beaudoin
`process?
`
` A: No, Dr. Gundersen heated the samples using a technique inconsistent with
`Beaudoin I and II. Specifically, Gundersen placed a heat block inside the oven of
`a gas chromatograph set to either 70°C or 125°C for at least one hour. He then
`used the heat block to heat vials of krill oil extract for 15 minutes at 125°C or 5
`minutes at 70°C. After Gundersen heated the vials, they were allowed to cool to
`room temperature before analysis.
`
`161. Q: What is the significance, if any, of Gundersen’s use of a heat block?
`
`A: Gundersen’s heating method was mediated primarily by air-liquid convection
`and not conduction. This treatment would not allow the oil to be heated the
`temperatures disclosed in Beaudoin I or II, or for the amount of time specified in
`Beaudoin I or II, due to the slow heat transfer to the oil from the heat block.
`
`162. Q: Is the distinction between convection and conduction heating accepted in
`the field?
`
`A: Yes, it is a basic and well-established fact that conduction results in much
`quicker heat transfer than convection.
`
`163.
`
`Q: Why is that?
`
`A: In simple terms, heated air contains relatively fewer molecules that can
`transfer heat from one object to another, as compared to heated liquids, such as
`oils as in a heated oil bath. As a result, the transfer of heat by convection is much
`slower than conduction.
`
`164. Q: Could you further explain this distinction by using an analogy?
`
`A: Yes, I frequently use analogies in teaching my students. To visualize
`convection heating, as used by Gundersen, consider putting your hand in a heated
`kitchen oven set to say, 400°F, which is about 200°C. Contrast this with putting
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`your hand in pot of boiling water (which is around 100°C), which would be akin
`to conduction heating. Even though the oven is set to a much higher temperature,
`putting your hand in the oven wouldn’t cause discomfort or injury immediately,
`but putting your hand in the boiling water would cause an immediate and painful
`burning sensation.
`
` Q: Would Gundersen’s use of a convection heating as opposed to
`165.
`conduction heating have affected the composition of the post-heated extracts?
`
`A: Yes. Gundersen’s heating was essentially ineffective and milder than the
`heating step taught in Beaudoin I and II because the heat block would not have
`maintained the temperature of 125°C for 15 minutes or 70°C for 5 minutes.
`Therefore, there would have been significantly less hydrolysis of the ester bonds
`than there would have been if Gundersen had heated using a water or oil bath, as
`has been done in other recreations commissioned by Aker such as those done by
`Dr. Budge.
`
`166. Q: Have you seen any evidence to support your conclusion that Gundersen’s
`use of the heat block would have been ineffective?
`
`A: Yes. The HPLC-MS data presented in Appendix A to the Gundersen
`Declaration, RX-0089, appears to detect the same intensity peaks for non-heated,
`heated to 60°C or 70°C, and heated to 125°C. This is shown by looking at the
`chromatograms labeled P308-1, P308-2, and P308-3. One would expect to see
`differences in the intensity of the peaks, for example, depending on whether it
`was unheated or heated to 125°C. This further underscores the ineffective heating
`approach used by Gundersen.
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`199. Q: You mentioned adding steps to Beaudoin. How did Dr. Budge’s sample
`creation deviate from Beaudoin I and II in this regard?
`
`A: Beaudoin discloses substantial moisture content in his krill oil. But Dr.
`Budge’s extraction process involved substantial additional water removal steps
`that were not performed in Beaudoin I or II. In particular, Dr. Budge explains at
`RX-0602.0013 that she heated the samples to 38°C during reduced-pressure
`evaporation and further explains at RX-0602.0014 that she used a separatory
`funnel and centrifuge. None of these water-removal methods was disclosed in
`Beaudoin I or II, and each method would independently result in a lower water
`concentration than would be present in a sample prepared according to Beaudoin I
`and II. This is an obvious change to the composition of the resulting samples, and
`it would necessarily affect the amount of hydrolysis and skew the results for at
`least some of the tests Respondents ran on the Budge Samples.
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`218. Q: To summarize, what is your opinion regarding these water removal steps?
`
`A: Individually and in combination, these water removal steps are deviations from
`the disclosed method of Beaudoin I and II. Used in combination, these additional
`water removal steps would result in samples having substantially lower water
`concentration than would be present in a sample prepared according to Beaudoin,
`which was reported to be about 10%. The results of Respondents’ tests on those
`samples are therefore skewed, and those results cannot be said to represent
`Beaudoin.
`
`Further, Dr. Budge’s use of additional water removal measures is rendered even
`more inappropriate in light of Beaudoin’s express teaching at RX-0163 at
`AKER877ITC00119430 that “[v]ariations between results from acetone
`extractions are mainly due to the water-oil separations.”
`
`As a result, it is my opinion that the results of any testing based on the Budge
`Samples are unreliable.
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`219. Q: You’ve generally referred to the problem of the Budge Samples having a
`lower water concentration. Why is this difference in water concentrations
`problematic?
`
`A: The absence of proper water-and-volatiles concentration in the Budge Samples
`renders unreliable tests run on the Budge Samples for at least two reasons. First,
`as I’ve explained, variations in water concentration from what is disclosed in
`Beaudoin I will impact the occurrence of hydrolytic degradation (i.e., hydrolysis)
`in the Budge Samples.
`
`220. Q: How does this relate to your criticism of the Budge Samples?
`
`A: The removal of additional water, as was done in preparing the Budge Samples,
`will decrease hydrolysis to a rate lower than was seen under Beaudoin I and II.
`Further, assuming that the Budge Samples have a lower free fatty acid content
`than the samples disclosed in Beaudoin, hydrolysis would further be suppressed.
`For this reason, the Budge Samples are unreliable for determining the w/w% of
`phospholipids in samples created according to Beaudoin I and II, since that
`percentage can be affected by hydrolysis.
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`227. Q: You previously said that the lower water concentration in the Budge
`Samples renders unreliable tests run on those Budge Samples for at least two
`reasons. What is the second reason?
`
`A: The water-and-volatiles concentration in the Budge Samples will necessarily
`affect the by-weight (i.e., w/w %) concentrations of phospholipids and omega-3
`fatty acids in those samples, and those concentrations are relevant to claims
`including claims 2, 3, 25, 26, and 94 of the ’351 patent and claim 1 of the ‘675
`patent. For example, a 100-gram sample having 35 grams of phospholipids and
`10 grams of water would have a phospholipid concentration of 35% w/w.
`However, if 8 grams of water are then removed (e.g., by evaporation through
`increased heat and/or use of a separatory funnel or centrifuge for separation), the
`sample would then have 35 grams of phospholipids out of a 92-gram sample,
`resulting in a phospholipid concentration of approximately 38%. Thus, for this
`additional reason, the total phospholipid calculations done by Dr. Moore and the
`omega-3 fatty acid calculations done by Dr. Lee on the Budge Samples do not
`accurately report the composition of samples prepared according to Beaudoin I
`and II.
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`248. Q: What caused this situation?
`
`A: It is unclear. Dr. Moore reported and stated during his deposition that a number
`of the Budge Samples had very low phospholipid levels. Dr. Brenna states at RX-
`0572C.0083 that, for the first set of Euphausia superba Budge Samples, meaning
`BEA-S0, BEA-S1, BEA-S2, the “results that were reported by Dr. Lee and Dr.
`Moore indicated that there was something wrong with these samples” and that
`“the results made absolutely no sense.”
`
`Also, I note that while Dr. Budge appears to have substantial experience
`extracting marine oils, her credentials do not indicate that she had ever extracted
`oil from krill prior to this assignment. Her lack of experience with krill is one
`possibility because, as Enzymotec wrote at CX-0810 at NEP877ITC-0064838, the
`“unique and sensitive components” of krill oil necessitate that it be handled in a
`fundamentally different way than fish oil.
`
`249. Q: How have Respondents addressed this situation?
`
`Fully one-third of the Budge Samples were deemed anomalous by Dr. Brenna in
`his report, and Dr. Brenna stated that he did not rely on them. These one-third of
`the Budge Samples also were not tested by Dr. Van Breemen.
`
`250. Q: In your opinion, is this a proper response to this situation?
`
`A: No, I disagree with Respondents’ approach. These allegedly anomalous
`Budge Samples constitute one-third of all the Budge Samples. Dr. Brenna
`identifies no scientific basis-statistical or otherwise-for simply disregarding one-
`third of the created samples simply because they demonstrate results that are
`surprising or unreasonable to him. Indeed, scientific inquiry requires
`investigating such surprising results rather than ignoring them.
`
`However, I am not surprised that Respondents’ experts encountered difficulty in
`preparing and analyzing the Budge Samples, given their inexperience in
`extracting oil from krill and the unique challenges in doing so.
`
`(d)
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`Other Deviations from the Methods Disclosed in
`Beaudoin I and II
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`1.
`
` “suitable for human consumption”
`
`Q: I’d now like to turn to the final limitation of claim one, “wherein
`375.
`the extract is suitable for human consumption.” In your opinion, does
`Beaudoin II disclose an extract that is suitable for human consumption?
`
`A: No, Beaudoin II does not disclose an extract suitable for human consumption.
`
`Q: What is the basis for your opinion that Beaudoin II does not
`377.
`disclose an extract suitable for human construction?
`
`A: As Dr. Brenna says, and I agree, Beaudoin I and II disclose essentially the
`same extraction process, so we can assume that the composition tables in
`Beaudoin I would apply to samples prepared according to the Beaudoin II
`process.
`
`Table 13 of Beaudoin I indicates that Beaudoin’s fractions contain a high level of
`remaining solvent and moisture, specifically, 10.0 and 6.8% for fractions I and I,
`respectively. As I explained before, these levels of solvent and moisture would
`render the oil not suitable for human consumption.
`
`Q: Did you take into account Beaudoin II’s statement that Dr.
`379.
`Beaudoin “tasted” the krill lipid fractions?
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`A: Yes. As I said earlier during our discussion of Beaudoin I, this anecdotal
`reporting of a single ingestion or tasting is by no stretch of the imagination
`evidence that the extracts were in fact suitable for human consumption. Any
`person of ordinary skill, or indeed, anyone applying common sense, wouldn’t
`conclude that a product is suitable for human consumption just because someone
`tried it once and didn’t suffer some kind of serious adverse health event. The idea
`of something being fit or appropriate for a human to eat or use contemplates the
`possibility of repeated or even regular use, for example, in the case of a dietary
`supplement.
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`Q: Let’s now move on to the next limitation in claim 1, which requires
`649.
`that the extract contain the claimed phospholipids. Does Fujita expressly
`disclose the claimed phospholipid?
`
`A: No. Fujita does not expressly disclose the presence of the claimed
`phospholipid in a krill extract. There is no disclosure in Fujita of any
`phospholipid with EPA and/or DHA attached, let alone with EPA and/or DHA
`concurrently attached at both the sn-1 and sn-2 positions. To the contrary, Fujita
`teaches away from obtaining an extract that contains the claimed phospholipid.
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`Q: How does Fujita teach away from obtaining an extract that
`650.
`contains the claimed phospholipid?
`
`A: As I mentioned earlier, Fujita’s goal is to obtain purified astaxanthin oil. To
`achieve this, it teaches removal of phospholipids and other lipids extracted from
`the krill along with the astaxanthin by heating and other methods.
`
`Q: What other techniques are taught by Fujita for removing
`653.
`phospholipids and other lipids, besides astaxanthin, from the extract?
`
`A: Fujita also calls for application of lipases.
`
`654.
`
`Q: What are lipases?
`
`A: Lipases are enzymes know to induce enzymatic hydrolysis.
`
`Q: Is enzymatic hydrolysis similar to the heat-induced hydrolysis
`655.
`process you explained earlier during our discussion of Beaudoin?
`
`A: Yes. Enzymatic hydrolysis is induced by enzymes, as opposed to heat, but it
`results in the same rupture of ester bonds that bind fatty acids to the glycerol
`backbone of the phospholipid.
`
`Q: Does Fujita utilize any other techniques that would degrade
`656.
`phospholipid?
`
`A: Yes, Fujita uses saponification, a very harsh technique that requires the use of
`caustic alkali in order to hydrolyze ester bonds in lipid and thus release free fatty
`acids and glycerol backbone. Although saponification is very useful to purify and
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`concentrate krill carotenoid pigments, as Fujita intends, it completely destroys
`phospholipids.
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`665. Q: Let’s first discuss Dr. van Breemen’s Fujita Hexane and Fujita Hexane-
`Ethanol work. For this method, in what ways did Dr. van Breemen’s sample
`recreation deviate from the disclosure of Fujita?
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`A: Let me first note that my critiques of Dr. van Breemen’s recreation of the
`Fujita Hexane method also apply equally to his recreation of the Fujita Hexane-
`Ethanol method. and the reverse is also true.
`
`One significant difference concerns the input material used. In his expert report.
`Dr. van Breemen did not identify or characterize the krill meal used in his
`experiment. exce t to indicate that he received it from Aker. He later confnmed
`
`that it was precursor material from which Aker
`
`manufacturest e Super aTM Kri 01 t at it sells for human C01lS1l111pllO11.
`
`E has substantiall different characteristics than does the whole krill
`mea use inFu'ita.
`
`differences demonstrate that Dr. van Breemen was using a fundamentally
`different starting material than was used in Fuita. rendering his
`lll oited
`recreation a failed recreation of Fuita.
`
`And Dr. van Breemen confumed dining his deposition that he did
`not c aracterize the krill meal he received and used. either.
`
`666. Q: Are you aware that Dr. van Breemen contends in his supplemental report
`that the difference in starting material would make no difference regarding the
`extractions or testing performed by Respondents?
`
`A:Yes.
`
`Q: Do you agree with Dr. van Breemen?
`
`A: No. I disagree. I cannot predict all the impacts that this deviation would have.
`but I am certain that it would influence the composition and uali
`of the
`resulting extract. For example. Aker carefully prepares
`to be used
`to make high— uali
`oil suitable for human consumption. and this careful
`preparation
`likel
`results in a lower concentration of free fa
`acids and water content.
`
`. B11t we do not know whether the sotu‘ce material
`
`used in Fujita was prepared in a similarly careful manner. The Fujita experiments
`were conducted approximately 30 years ago. when the equipment and methods
`used by Respondents and the knowledge of lipid and phospholipid hydrolysis
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`were not as readily available as they are now. The krill meal used in Fujita would
`likely have had a substantially higher concentration of free fatty acids, in which
`case the resulting extract would also be expected to have a higher free fatty acid
`concentration.
`
`668. Q: Are there other differences between what Dr. van Breemen did and the
`Fujita Hexane and Fujita Hexane-Ethanol methods?
`
`A: Yes. According to Fujita, the proper ratio of vessel volume to the volume of
`extraction solvent was 1.5 – 300 liters to 200 liters – but Dr. van Breemen used a
`ratio of 2.667 – 2 liters to .75 liters. This difference is significant, because it
`provides a larger mixing volume for the Breemen recreation. The larger mixing
`volume will cause a more effective mixing of the extraction mixture, and result in
`a more effective extraction. The further effects this would have are unknown, but
`Dr. van Breemen’s failure to follow the teaching of Fujita further renders his
`purported recreation of Fujita unreliable.
`
`669. Q: Are there still other differences between what Dr. van Breemen did and
`the Fujita Hexane and Fujita Hexane-Ethanol methods?
`
`Yes. One step in the Fujita Hexane and Fujita Hexane-Ethanol methods requires
`the residue to be “washed three times using an equivalent amount of solvent.”
`RX-0204 at AKER877ITC00803132. The proper ratio of extraction volume to
`wash volume is 1.667, meaning that 200 liters of solvent were used for extraction
`and three portions of 40 liters of solvent were used for washing. But Dr. van
`Breemen used a ratio of .333, as he used 750 milliliters of solvent for extraction
`but three portions of 750 milliliters of solvent for washing. Dr. van Breemen’s
`incorrect usage of proportionately much more solvent for the wash resulted in a
`more exhaustive extraction than in Fujita. Dr. van Breemen did not adjust the
`solvent removal step to account for the increased volume of solvent added with
`successive washes. Since he failed to adjust for it, then additional solvent would
`remain in the extract. The result is an unfaithful recreation of Fujita, and one that
`is even more unsuitable for human consumption
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`672. Q: What does Dr. van Breemen mean when he refers to scaling down his
`experiments for the Fujita Hexane and Fujita Hexane-Ethanol methods?
`
`A: This is another problem with Dr. van Breemen’s Fujita recreations. Dr. van
`Breemen acknowledges that his recreation of the Fujita Hexane and Fujita
`Hexane-Ethanol methods differ from Fujita because he is performing a scaled-
`down version of the Fujita extraction methods. Specifically, Fujita used 200 liters
`of solvent and 40 kilograms of krill meal as starting materials, and performed the
`washing step three times using 40 L of solvent. In contrast, Dr. van Breemen
`used 750 ml solvent and 150 gram krill meal.
`
`673. Q: Do you understand that Dr. van Breemen in his supplemental report and
`Dr. Brenna in his witness statement contend that this scaling would not impact
`the Fujita extractions?
`
`A: Yes.
`
`674. Q: Do you agree with them?
`
`A: No. The impact is significant but not entirely predictable. Dr. van Breemen
`and Dr. Brenna say that the scaling down of Dr. Van Breemen’s experiments did
`not affect the results or their opinions. Dr. van Breemen also alleges that the Fujita
`Reference teaches that small-scale experiments are appropriate for testing the
`same extraction methods using larger extractors. To support his arguments, Dr.
`van Breemen cites to Fujita’s teaching with respect to the model extraction tests.
`Specifically, Fujita states at RX-0204 at AKER877ITC00803140 that:
`
`[M]odel extraction tests were performed using a small-scale glass column, and
`then extraction tests were performed using an oil plant once-through pilot
`apparatus in order to determine the appropriateness of once-through extraction.
`
`But I disagree. Indeed, Dr. van Breemen mischaracterizes the teachings of Fujita.
`To the extent that Fujita teaches “scaling down” of experiments, Fujita also
`explicitly teaches that large-scale extractions require distinct experimental
`conditions from small-scale extractions. Therefore, Fujita teaches scaling up from
`a small-scale extraction to a large-scale extraction. Dr. van Breemen, however,
`does the opposite. His purported recreation is from a large-scale extraction such
`as in Fujita to Dr. van Breemen’s small-scale extraction. One cannot assume that
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`these extractions will be similar because scaling extractions in either direction
`presents unexpected challenges. This is further evidenced in the Bergelson
`reference – a reference supplied by Respondents – which teaches at RX-
`0189.0007that “[s]caling up of such micromethods presents new unpredicted
`problems.”
`
`676. Q: Let’s now discuss Dr. van Breemen’s Fujita Once-Through work. For
`this method, in what ways did Dr. van Breemen’s sample creation deviate from
`the disclosure of Fujita?
`
`A: As one example, the raw material used by Dr. Van Breemen differs from what
`is taught by Fujita, and these differences could have unpredictable effects on the
`resulting extracts.
`
`679. Q: Are there other differences between what Dr. van Breemen did and the
`Fujita Once-Through method?
`
`A: Yes. Significantly, Fujita does not teach solvent removal using the once-
`through method. And the solvent removal conditions employed by Dr. van
`Breemen, 30(cid:113)C under a stream of dry nitrogen, are inconsistent with even the
`solvent removal conditions that are taught by Fujita, which were 70(cid:113)C and 40 Torr
`for the Fujita Hexane and Fujita Hexane-Ethanol methods. By using much lower
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`temperature for solvent removal, Dr. van Breemen likely reduced hydrolysis,
`while dry nitrogen created an inert atmosphere during solvent removal. The inert
`atmosphere likely reduced lipid oxidation including oxidation of fatty acids,
`particularly oxidation-sensitive EPA and DHA. These significant deviations
`during solvent removal likely caused compositional differences in the extract.
`
`680. Q: Do you understand that Dr. van Breemen contends in his supplemental
`report that it would be reasonable and appropriate to use a stream of nitrogen in
`a warm bath to remove solvent and that he would expect to find the claimed
`phospholipids even if he had heated Fujita once-through to a higher
`temperature?
`
`A: Yes.
`
`681. Q: Do you agree with Dr. van Breemen?
`
`A: No. First, regardless of what is reasonable and appropriate, Dr. van Breemen’s
`use of a stream of nitrogen in a warm bath simply is not disclosed for the Fujita
`once-through method.
`
`682. Q: Would it have made a difference in terms of detecting the claimed
`phospholipid in the van Breemen/Fujita Once-Through Samples if Dr. van
`Breemen had performed solvent removal for the Fujita once-through method
`under the same conditions as were applied for the other Fujita recreations?
`
`A: It might have. Dr. van Breemen can only speculate as to the outcome if he had
`applied more heat in performing his Fujita once-through experiment. In any event,
`Fujita does not even teach the use of 70(cid:113)C for the Fujita Hexane and Fujita
`Hexane-Ethanol methods until after water removal. So applying 70(cid:113)C to the
`Fujita once-through method, from which water had not been removed, may have
`caused greater hydrolysis than in his Fujita Hexane and Fujita Hexane-Ethanol
`experiments.
`
`(c)
`
`Lack of Composition Data
`
`683. Q: Do you have other criticisms of Dr. van Breemen’s application of the
`Fujita Once-Through method?
`
`A: Yes. When recreating an extraction method known in the art, one of skill in the
`art should compare the composition of the resulting extract, to the extent possible,
`to the composition of an extract known to have resulted from use of the extraction
`method being recreated. Indeed, Fujita disclosed numerous data concerning the
`composition of the krill extract created using that method.
`
`But Respondents’ experts have disclosed almost no comparable composition data
`concerning the van Breemen/Fujita Samples. This failure to disclose information
`confirming the composition of the van Breemen/Fujita Samples marks an absence
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`of proof that the van Breemen/Fujita Samples are accurate recreations of the
`Fujita methods.
`
`684. Q: Do you have any examples of data that could have been measured but was
`not?
`
`A: Yes. For example. Fujita discloses extraction and composition data including
`yield. lipid recovery rate. and percentages of polar and neutral lipids, for each of
`the hexane. hexane-ethanol. and once-through extractions. Measiuements of this
`data were not provided by Dr. van Breemen. nor were they provided by the other
`experts who tested the van Breemen/Fujita Samples.
`
`((1)
`
`Conclusions
`
`685. Q: In summary, then, what is your opinion concerning the van
`Breemen/Fujita Samples?
`
`A: In my opinion. the van Breemen/Fujita Samples are failed recreations of Fujita.
`and therefore testing of the Van Breemen/Fujita Samples does not indicate the
`composition of any extract created using the methods of Fujita.
`
`(3)
`
`Van Breemen Testing
`
`686. Q: What is your understanding of the testing performed by Dr. van Breemen
`on the van Breemen/Fujita Samples?
`
`A: Dr. van Breemen analyzed the three van Breemen/Fujita Samples for the
`presence of the claimed phospholipid species. And Dr. Brenna stated his belief
`that Dr. van Breemen tested properly and identified the presence of some of the
`claimed phospholipids in the tested samples.
`
`Q: Do you have an opinion about the tests performed by Dr. van Breemen?
`
`would have substantial concerns about some of the analysis disclosed by Dr. van
`Breemen. and I do have such concerns.
`
`Q: What are your criticisms?
`
`A: As I previously stated. Dr. van Breemen only selectively tested for the
`presence of the claimed phospholipid species. Although he tested the three van
`Breemen/Fujita Samples. he did not analyze all of the Budge Samples.
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`It is my opinion that Respondents’ decision not to perform each test on each of
`the purportedly recreated samples undermines their claim that certain measured
`results are inherent in the samples created according to Fujita.
`
`689. Q: In summary, then, what is your opinion concerning Dr. van Breemen’s
`testing?
`
`A: In my opinion, substantial doubt exists as to the reliability of certain aspects of
`the analysis that Dr. van Breemen performed to identify the presence of targeted
`phospholipids PC-EPA/EPA, PC-EPA/DHA, and PC-DHA/DHA. Further, as
`explained above, the unreliability of the Budge Samples, the van Breemen/Fujita
`Samples, the van Breemen/Rogozhin Samples, and the White Samples renders the
`analysis in Dr. van Breemen’s Report meaningless, since it was performed on
`samples that do not properly reflect the methods of Beaudoin I or II, Fujita, or
`Rogozhin.
`
`(4)
`
`Avanti Testing (Moore Report)
`
`690. Q: What is your understanding of the testing performed by Avanti?
`
`A: Avanti selectively analyzed the Budge Samples, the van Breemen/Fujita-
`Hexane samples, and the van Breemen/Fujita-Hexane-Ethanol samples for total
`lipids and phospholipids and free fatty acid content. But Avanti did not analyze
`the van Breemen/Fujita once-through samples. Dr. Brenna states that he
`confirmed that the proper analysis was done and that it was done properly.
`
`691. Q: Do you have an opinion about the tests performed by Avanti?
`
`A: I do not concur with Dr. Brenna. One of skill in the art would have substantial
`concerns about the methods and data disclosed in the Moore Report, and I do
`have such concerns.
`
`(a)
`
`Free fatty acid analysis
`
`692. Q: Do you have any criticisms of the methods and data disclosed by Dr.
`Moore regarding free fatty acid analysis?
`
`A: Yes. Dr. Moore only selectively tested free fatty acid data. For example, Dr.
`Moore reports free fatty acid numbers for only the van Breemen/Fujita Hexane
`samples and the van Breemen/Fujita Hexane-Ethanol samples while n