Source: SENSOR DEVELOPMENT CORPORATION submitted to
A NEW NANO-BASED DETECTOR FOR THE INDIAN MEAL MOTH, BOTH ADULT INSECTS AND LARVA
Sponsoring Institution
National Institute of Food and Agriculture
Project Status
TERMINATED
Funding Source
Reporting Frequency
Annual
Accession No.
1012558
Grant No.
2017-33610-26987
Project No.
OHOK-2017-00435
Proposal No.
2017-00435
Multistate No.
(N/A)
Program Code
8.5
Project Start Date
Sep 1, 2017
Project End Date
Apr 30, 2019
Grant Year
2017
Project Director
Smilanich, N.
Recipient Organization
SENSOR DEVELOPMENT CORPORATION
16651 W. SPRAGUE ROAD, SUITE C204
STRONGSVILLE,OH 441363
Performing Department
(N/A)
Non Technical Summary
The Indianmeal moth is the most common stored product insect found throughout the U.S. Adult Indianmeal moths can be found almost anywhere in the temperate regions of the world. In the U.S. and Europe it is the one insect pest that causes the most damage. The economic losses from these pests in processing, transporting and storing can be in the millions of dollars per contamination incident, product recall, consumer complaint/litigation, and pest control applications. Yet there is no efficient, low cost method to monitor and detect Indianmeal moths.The Indianmeal moth is most often found feeding on finished food products, the ingredients for food such as stored wheat products, milled/processed wheat, and other stored products such as milled cereal products, flour, bran, pasta products, spices or infesting equipment where food is prepared, processed, packaged or stored. Indianmeal moth larvae are the destructive life stage of the insect, eating voraciously. The larvae are highly mobile and continuously seek out new sources of food. While there are no direct health concerns, the psychological health of an individual knowingly consuming these larvae can have dramatic impacts and consequences including legal costs for the retailer, distributor or manufacturer of the product. It is the one insect found more often than any other on stored food and grain in the U.S.Over fifty years the genetics of this insect have changed to resist the commonly used pesticide Malathion. In the 1970's, the Indianmeal moth started showing signs of resistance to this insecticide. Since then, the Indianmeal moth has become the most resistant insect known to man. As the other insect competitors for the same habitat and food sources were slower to develop this genetic resistance to Malathion, the Indianmeal moth emerged as the primary pest of stored products. SDC's objective in this project is to develop an affordable and accurate device that can detect Indianmeal moth and Indianmeal moth larvae in stored products. The SDC device will provide early warning of insects in food processing and storage to help preventinfestation and control populations and drastically reduce the need for hazardous chemicals in the food industry. The primary goal of this project is to demonstrate the feasibility of SDC's innovative nano-tin oxide sensor to detect pheromones and semiochemicals, chemicals given off by insects to communicate with other insects. SDC will detect these chemicals simultaneously at very low levels and to differentiate between them and other gases in the air. SDC anticipates that if the project is successful the most damaging insect of stored products will be detected, and the size of their populations reported. The key technical benefit is a better quality reading of insect populations. This informs the pest manager of the best time to fumigate and prevents overuse of chemical fumigants. Today's usual procedure, trapping and counting insects in a discrete sample, then projecting a population for the total is subject to sampling error and could result in unnecessary fumigation.SDC's platform technology is based on the ability of its sensors to detect virtually any reducing gas with extremely high sensitivity, so the potential for follow-on applications is significant. SDC has plans to develop additional pheromone-based detection devices for other insects in the agricultural grain storage and stored products markets. Additionally, SDC recognizes the opportunities available to it and its potential corporate collaborators to use this technology for applications beyond agriculture such as medical diagnosis of pulmonary fungal infections, odor detection, monitoring indoor air quality, mold detection in residences and hospitals, and homeland security. It may be especially useful in this context for the federal government, which could use the device in forestry applications to locate termites that attack and destroy forests and forest products. Bed bug incidences are on the rise across the country, and there may be a need in the future for the government's application of SDC's technology to combat this pest. Federal buildings in Cleveland, Ohio, Washington D.C. and St. Albans, Vermont have had bed bug incursions. Finally, the federal government could use this highly sensitive, portable device to scan for explosives.
Animal Health Component
0%
Research Effort Categories
Basic
50%
Applied
30%
Developmental
20%
Classification

Knowledge Area (KA)Subject of Investigation (SOI)Field of Science (FOS)Percent
50350101130100%
Goals / Objectives
Sensor Development Corporation's (SDC's) goal is to develop an affordable sensor that enables pest monitoring and detection in an extensive number of venues where economics and health issues occur. This single portable unit will detect the Indianmeal moth adult insect and larvae below the targeted infestation number, allowing pest managers to take action to limit damage from these pests and contain them to specific areas early. This is done by detecting the Indianmeal moth adult female insect's sex pheromones and by sensing the semiochemicals in Indianmeal moth larvae frass and mandibular gland secretions.The Indianmeal moth is the most common stored product insect found throughout the U.S. It is the one insect found more often than any other on stored food and grain in the U.S. The adult Indianmeal moth can be found almost anywhere in the temperate regions of the world. In the U.S. and Europe it is the one insect pest that causes the most damage.SDC will accomplish this goal with the following objectives:In the laboratory SDC will modify their existing prototype device to detect adult Indianmeal moths and larvae by using basic and applied knowledge to change the onboard chips and their operating conditions. This will include evaluating various catalysts in the semiconductor material on the chips and various firing temperatures for the semiconductor.Further laboratory testing will include using toluene in the gas stream with the insect pheromones and larval semiochemicals to identify the best chips for selectivity. Toluene represents with the background interfering gases found in the insect environment.Demonstrate in a field trial that SDC device responds to live adult Indianmeal moths and to live Indianmeal moth larvae present in a typical stored product or products, such as soft white flour, whole wheat products and wheat bran productsConfirm presence of volatile semiochemicals and identify other volatiles in headspace gas over stored product with Indianmeal moth larvae. This work will also identify the physico-chemical properties of the Indianmeal moth larva semiochemicals.
Project Methods
The evaluation activities conducted and milestone timing are summarized in Chart IChart I: Evaluation Activities and Timing - Phase I Project 2017 2018 Evaluations Start End J J A S O N D J FSensor Chip Sensitivity Evaluation 6/1/17 7/31/17 --------Acquire and Tank Synthetic Larval 7/1/17 9/30/17 --------------Bench Test Sensor Chip Selectivity 10/1/17 12/31/17 ------------ Field Evauation with Live Insects 1/5/18 2/15/18 -----Evaluate Minimum Detection Level 11/1/17 11/30/17 -----Evaluate the Valatome over larvae 12/1/17 2/20/18 -----------Evaluation studies are conducted on nano-crystalline tin oxide particles made by sol-gel methods, fabricating sensor chips by microfabrication and thick-film techniques, assessing thesemiconductor film properties by optical and analytical methods, and evaluating sensor performance using a custom computerized testing apparatus. These evaluation studies are analyzed for sensor response data that describes the sensor chip sensitivity to relevant volatile semiochemicals and pheromones. Benchmarks for performance are sensitivities of 100 nanomhos/ppb to 175 nanomhos/ppb.The larva semiochemicals are not commercially available. Synthesis is being considered at three different locations. These pheromones and semiochemicals can be made into test gases in pressurized cylinders using a small amount of the material by a specialty gas supplier with whom SDC has developed a working relationship. The specialty gas supplier provides a pressurized cylinder containing 2 ppm of the gas in dry nitrogen. Lower concentrations (e.g., 50, 100, 150, 200 ppb) are prepared using a gas mixing manifold in SDC's laboratory. The 2 ppm specialty gas is mixed with the required amount of 100% dry nitrogen in the manifold to produce the desired lower concentration. Mixing is accomplished with precision, computer-controlled valves to meter the materials into a final gas stream which is injected into the prototype device. The field trials will be run exclusively using live adult Indianmeal moth pheromones and semiochemicals from live Indianmeal moth larvae as sources of marker gases.Success is measured by bench evaluation of the sensor using test gases and in field evaluation of the sensor detecting live insects. These measures are related to the detection of the insect and to the quantification of the number of insects and determination of the insects' stage of development, that is to say, larva or adult. By demonstrating the feasibility to design a fully functional device capable of commercial application, the project has a major impact on the pest management industry.Bench evaluations provide a correlation between the concentration of volatile semiochemicals and pheromones with chip response. Field evaluations provide a correlation between number of insects in the stored product and the chip response. This data allows use of chip response to determine the concentration of semiochemicals or pheromones and the number of insects in the stored product.The minimum detection level for high sensitivity chips will be evaluated. Benchmarks for performance are in the range of 500 parts per trillion to 1.5 parts per billion. SDC has experience with other insects in other projects achieving minimum detection levels in this range.The evaluations will be conducted on sensor chips fabricated using SDC in-house processes. These processes are: 1) making alumina chips with a platinum heater trace on one side and extended, interdigitated platinum contact traces on the other, the traces terminating in gold alloy connection pads; 2) producing water-based tin oxide gels by a sol-gel process; 3) doping transition metal catalysts into the gels to enhance response to various volatile organic compounds (VOCs); 4) spin-coating the tin oxide gels uniformly onto the alumina chips; 5) drying/calcining the gel to produce a nanocrystalline semiconductor layer... the layer's resistance changes when reducing (electron-donating) gas phase VOCs contact its porous, high area surface; 6) wire-bonding to connect the chip to a holder, suspending the chip to achieve thermal isolation while allowing connection to electronics that controls its operation and processes the chip's signal. SDC developed methods for making sol-gels containing any one of seven metals: palladium, tungsten, platinum, molybdenum, ruthenium, nickel and osmium. These catalysts enhance the chip's response to specific gases, enabling selective detection of gas markers of different bio processes. SDC designed and built a prototype including electronics, microprocessor, and programming needed to control the chips and collect the chip response in a digital text file ready for analysis. Six operating channels can be run at temperatures from 200oC to 400oC. This prototype forms the basis for many different products.Efforts - Informal or Formal EducationWe intend to file patents on our technical advances. The Specification of the patent is a valid way to promulgate scientific knowledge to the technical, business and general community. It is important for members of those communities to have a resource to understand how practical devices work, and the engineering and scientific fundamentals on which those devices are based.

Progress 09/01/17 to 04/30/19

Outputs
Target Audience:During this reporting period, SDC reached out to a number of commercial entities in the pest control services industry and commercial entities involved in storage, handling and processing of food ingredients and food products. SDC's objective was to inform these commercial firms of the advantages of SDC's electronic sensor product compared to the present techniques used to monitor insect and larva activity in their stored products. SDC's final objective was to gain acceptance of our concept by these commercial entities and achieve their written support for our efforts. SDC succeeded in gaining Letters of Support from Insects Limited, Inc., Copesan, The Stafford County Flour Mill Co., Lundberg Family Farms, The California Walnut Board and the California Dried Plum Board. SDC visited Lundberg Family Farms. Nestle U.S.A., Archer Daniels Midland (rice milling), Mars, Inc., Bayer (crop sciences), The California Almond Board and J.P. Morgan (ship and rail transport of food products) are also members of SDC's target audience. SDC visited Archer Daniels Midland's rice milling operation near Sacramento, California SDC also has letters from the USDA ARS San Joaquin Valley Agricultural Sciences Center and from Insects Limited, Inc. confirming their intent to collaborate with SDC on a Phase II SBIR project which SDC has proposed to NIFA. Changes/Problems:A change was made to Technical Objective 3. In the proposal as awarded, the objective was stated as follows: Technical Objective 3: Confirm presence of volatile compounds in headspace gas over stored product with IMM larvae. Technical Objective 3 had two subordinate Tasks: Task 1: What is the volatome of gases over stored product with IMM larvae present? Task 2: What are the physico-chemical properties of the IMM semiochemicals? Task 1 has been expanded to include the larva and cocoon volatome. It is being completed and is being reported in the Accomplishments section of the final report on the REEport Portal. Task 2, characterization of the synthesized semiochemical materials, was planned to quantify what was expected to be a very low gas phase concentration in the event that it was not possible to get the material into pressurized tanks for lab system testing. But, the material was successfully containerized. So, resources were reprioritized away from this work and the field trial was expanded to include sensing and quantifying pupae in cocoons on the recommendation of SDC's USDA collaborators. What opportunities for training and professional development has the project provided?The project gave a UC Davis PhD student working at USDA ARS Parlier, CA an opportunity for new innovative means of identifying larval biomarkers and to work with an industrial commercial partner. How have the results been disseminated to communities of interest?SDC has communicated results of the field trial by close collaboration effort with USDA ARS personnel at the Parlier, CA station. What do you plan to do during the next reporting period to accomplish the goals? Nothing Reported

Impacts
What was accomplished under these goals? Acquired adult, larval Indianmeal moth (IMM) marker VOCs in suitable form for lab work. Insects Limited, Westfield, IN synthesized 9,12-tetradecadienylacetate, adult female IMM pheromone. SDC made it into a test gas, 2 ppm in dry N2 cylinder to use in SDC's lab test system. Round 1 chip response work used a commercially available surrogate for the semiochemicals in larva saliva, feces, frass. SDC's USDA collaborators (San Joaquin Valley Station, Parlier, CA) synthesized one of the larval semiochemicals. This work was done under an SDC CRADA with USDA ARS Parlier. SDC made the semiochemical into a test gas, 2 ppm in dry N2 cylinder for Round 2 work. 2. Selected un-catalyzed and catalyzed tin oxide sensor chips for testing; devised/applied ways to enhance chip sensitivity and selectivity. Lab Work to Select Chips: SDC's available chips are un-catalyzed chips and chips doped with catalysts, 8 total options. Sensitivities were defined by injecting 200 ppb of IMM pheromone or semiochemical in air onto each chip and computing the conductance change per change in analyte concentration: the Specific Net Conductance, SNC (nanomhos/ppb). Chip production process changes and post-production treatments were evaluated to enhance performance and stability. "Two-gas" experiments addressed sensitivity and selectivity. Round 1 used an un-catalyzed and a catalyzed chip with the adult pheromone and the surrogate larval semiochemical. Round 2 used an un-catalyzed chip and a catalyzed chip and an un-catalyzed chip with a second catalyzed chip; analytes were the adult pheromone and the synthesized larval semiochemical. SDC's concentration calculation uses the idea that each chip responds to each analyte independently. Chip conductance with multiple analytes is the sum of these contributions. The chip sensitivity to one analyte (the SNC), measured for each gas/chip pair before the chips are put into service, is used to compute the contribution of each analyte. Analyte concentrations (correlated to insect count) are calculated using well-known math techniques. The two gas lab experiments used this method. The Round 1 capping run with adult pheromone and surrogate larval semiochemical showed that an un-catalyzed chip and the first catalyzed chip can detect the adult pheromone and surrogate larva semiochemical. The expected concentration of both analytes is 100 ppb. Three replicate runs gave (pheromone/semiochemical) concentrations of (67/23), (74/19), and (83/79) ppb. The Round 2 capping run with adult pheromone and synthetic semiochemical showed that an un-catalyzed chip paired with the second catalyzed chip and with the first catalyzed chip can detect the adult pheromone and synthetic larva semiochemical selectively. The un-catalyzed chip and second catalyzed chip gave (pheromone/semiochemical) concentrations of (48/99) ppb when (100/100) ppb were expected. Un-catalyzed chip and the second catalyzed chip gave (pheromone/semiochemical) concentrations of (68/36) ppb when (100/100) ppb were expected. Conclusion: adult pheromone and larval semiochemical can be sensed selectively in the presence of the other analyte with un-catalyzed, and catalyzed chips. Additional two-gas experiments were run. Uncatalyzed chip SNCs (nanomhos/ppb) averaged 65.6+13.6 for the larva synthetic semiochemical and 178.5+16.1 for adult pheromone. The first catalyzed chip SNCs averaged 3.42+0.83 for the larva synthetic semiochemical and 7.61+0.41 for adult pheromone. Calculated (semiochemical/pheromone) concentrations using average SNCs and sensor signals when the two analytes were injected simultaneously at 100 ppb gave the following ppb concentrations for 6 runs: (207/108), (22/191), (108/152),(133/100), (100/181), (90/138). Conclusion: the electronic device provides information accurate enough for warehouse or bin managers to make decisions about taking action before larva/insect infestations occur. Ran successful field trial to show prototype capability with live insects, larvae and cocoons. The sensor chips used were un-catalyzed, and two catalyzed chips. Table 1 shows SNCs. Table 1: Sensitivities of chips (SNCs) for Marker Compounds No cat-Chip Chip-calyst 1 Chip-catalyst 2 Marker Volatile Adult Pheromone 184 74 272 Larval Semiochemical 80 37 142 The USDA Parlier, CA trial used a "reference" pail of clean flour always free of insects, and a "sample" pail of clean flour with stored product insects inserted. Jars of 5, 20, and 75 adult female IMM, IMM larvae and IMM larvae in cocoons were used. USDA's entomologist provided the insects and larvae, ensuring that they were the right sex and healthy. A fourth jar of each stage was provided to test the predictive ability of SDC's sensor. The entomologist knew the count, SDC workers did not. Adjusting a T-valve connecting the pails to SDC's prototype to sample headspace gas from the "reference" pail with "clean" flour determined a baseline resistance. Meanwhile, insects were put into the "sample" pail. Then, the T-valve was switched to the "sample" pail. Its resistance was used with the baseline resistance to calculate a Net Resistance. This sequence was repeated for insects introduced in the following order and number: 5, 25 (5+20), 100 (5+20+75). This was done for adult insects, larvae and for larvae in cocoons. Net Resistance was correlated with the counts of adults, larvae and larvae in cocoons. Insect, larva and cocoon counts were predicted from curves correlating the resistance change from the reference pail to the sample pail to larvae, cocoon or adult insect counts. The data fit to a mathematical curve. The curves allow computation of unknown larva, cocoon or adult counts from known resistance changes. Also, "blind test" predictions are shown. These are the counts of larvae, larvae in cocoons and adult female moths predicted using SDC's correlation with "blind" samples provided by the USDA entomologist as described in the description of the experiment. Table 2 comparing these computed counts to the known counts shows the correlation to be very good. Table 2: Correlation of Prototype signal to Larvae, Cocoons, Insect Count Live Larvae Cocoons Adult Females Chip Known Predicted Known Predicted Known Predicted 5 10 5 4 5 5 Pos #2 - 25 26 25 25 no reading no reading Uncatalyzed 100 52 100 99 100 75 Blind Test 150 304 150 123 75 51 Variation is seen at very low analyte concentration with live larvae. Live larvae are over estimated in the blind test. Adult moths are under estimated. Live insects and larvae produce amounts of semiochemicals that vary with time of day, expected to be less consistent than flow from lab gas cylinders. Technical Objective 3, Task 1 defining the larvae and cocoons volatome is in progress. A peak consistent with 4-hydroxy-2-oleoylcyclohexane-1,3-dione was observed in GC/MS. This 393 mass/charge peak has a retention time slightly longer than 2-oleoylcyclohexane-1,3-dione, consistent with that reported in Howard & Baker, Comp.Biochem.Physiol.,Part B 138 (2004)193-206. 4-Hydroxy-derivative synthesis is underway as are other analytical methods to confirm identification. Technical Objective 3, Task 2 was planned to quantify the gas phase concentration of a high molecular weight semiochemical, expecting that it lacked the vapor pressure to be containerized and detected. This became moot when the material was successfully containerized and detected. Resources were shifted from this work to field trial activity and analysis sensing cocoons.

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