Cottonseed Samples Research Articles

Changes in cottonseed meal quality during post-harvest processing of cottonseed

This study investigates aflatoxin contamination levels during the post-harvest processing of whole cottonseed into defatted cottonseed meal, a critical feed component in the dairy industry. Whole fuzzy cottonseed, a byproduct of cotton gins, undergoes various processes to extract oil and produce meal and hulls. These are either used as animal feed or soil amendments. However, aflatoxin contamination poses significant challenges due to strict FDA action levels for dairy and beef cattle feed. This contamination occurs when Aspergillus flavus infects crops under specific environmental conditions or through improper handling during post-harvest processes. Our research aims to document aflatoxin levels during each stage of post-harvest processing, from cleaning to meal formation. Preliminary findings suggest that certain stages may concentrate aflatoxins akin to other agricultural products like dried distillers’ grains and solubles (DDGS). The implications of these findings could be profound for the dairy industry, where low allowable aflatoxin levels impact both economic and animal health outcomes. The cottonseed post-harvest process consists of cleaning, delinting, hull removal, kernel flaking, oil extraction, and meal formation. Understanding how aflatoxin levels change during these steps is crucial for ensuring safe and high-quality defatted cottonseed meal for livestock consumption. Microbial levels increased by 4 orders of magnitude during the acid delinting process, from 7.0× 105 to 5.2 × 109 CFU/g, and 5 orders of magnitude during the mechanical delinting process, from 7.3× 105 to 1.5 × 1010 CFU/g for the inoculated cottonseed samples. Higher microbial load was associated with lower protein levels and lower fat acidity levels. Further research will shed light on the effects of aflatoxin concentration on the nutritional value of the final product.

Near-Infrared Spectroscopy Analysis of the Phytic Acid Content in Fuzzy Cottonseed Based on Machine Learning Algorithms.

Cottonseed is rich in oil and protein. However, its antinutritional factor content, of phytic acid (PA), has limited its utilization. Near-infrared (NIR) spectroscopy, combined with chemometrics, is an efficient and eco-friendly analytical technique for crop quality analysis. Despite its potential, there are currently no established NIR models for measuring the PA content in fuzzy cottonseeds. In this research, a total of 456 samples of fuzzy cottonseed were used as the experimental materials. Spectral pre-treatments, including first derivative (1D) and standard normal variable transformation (SNV), were applied, and the linear partial least squares (PLS), nonlinear support vector machine (SVM), and random forest (RF) methods were utilized to develop accurate calibration models for predicting the content of PA in fuzzy cottonseed. The results showed that the spectral pre-treatment significantly improved the prediction performance of the models, with the RF model exhibiting the best prediction performance. The RF model had a coefficient of determination in prediction (R2p) of 0.9114, and its residual predictive deviation (RPD) was 3.9828, which indicates its high accuracy in measuring the PA content in fuzzy cottonseed. Additionally, this method avoids the costly and time-consuming delinting and crushing of cottonseeds, making it an economical and environmentally friendly alternative.

Raman spectroscopic assessment of fibers and seeds of six cotton genotypes

AbstractRaman spectroscopy (RS) is a vibrational spectroscopy. This work reported the RS spectral characteristics of fiber and seed of six cotton (Gossypium sp.) genotypes differing in fiber length. While the RS spectra of fiber samples were dominated by the cellulose‐related peaks, the spectra of cottonseed samples were featured by the bands related to oil, protein, carbohydrate, and lignin components. Principal component analysis (PCA) revealed that the first two principal components (PCs) accounted for >87% of the total variation of the two types of samples. The PC1 versus PC2 plot classified the six fiber samples into three groups, but their cottonseeds into four groups. This experimental evidence implied the possibility of RS combined with PCA for rapid fiber phenotyping of cotton as well as for evaluating cottonseed nutrient information.

Paper-Based Simplified Visual Detection of Cry2Ab Insecticide from Transgenic Cottonseed Samples Using Integrated Quantum Dots-IgY Antibodies.

In the present study, an easy to use field-deployable methodology was developed for onsite detection of pesticidal crystal protein Cry2Ab from transgenic cotton crops to reduce seed adulteration. Anti Cry2Ab IgG and IgY antibodies were developed against recombinant Cry2Ab protein in New Zealand white rabbits and in white leg horn chickens, respectively. Carboxyl-functionalized CdTe quantum dots (QDs) were used as revealing probes, and nitrocellulose paper was used as an assay matrix. Recombinant Cry2Ab was generated in the lab and used for immunization of chicken and rabbits. After successful immunization and attaining the desired titer values (1:32 000 for IgY and 1:64 000 for IgG), eggs and hyperimmune sera were collected. Anti Cry2Ab IgY was purified as per the standardized protocols, and anti Cry2Ab IgG was purified using protein A affinity chromatography. Sensitivity of the generated antibodies was examined using indirect ELISA methods against recombinant Cr2Ab protein. Specificity evaluation was carried out against other Cry proteins including Cry2Ab, Cry4b, Cry4a, Cry1Ec, and Cry1Ac. Functionalized CdTe QDs were characterized for structure and shape as well as fluorescence properties using standard laboratory techniques. A field-deployable paper-based detection methodology was developed where IgG acted as the capturing antibody and IgY-linked CdTe QDs were used as revealing probes. The limit of detection (LOD) and quantification (LOQ) were found to be 2.91 ng/mL and 9.71 ng/mL, respectively. The effect of matrix interference was assessed on the different plant crude extracts of cottonseed materials.

Preliminary study on discrimination of transgenic cotton seeds using terahertz time-domain spectroscopy.

Presence of genetically modified (GM) organisms is considered to be controversial by legislation and public. It is very important to develop detection methods for early discriminations. Conventional gene detection methods, including protein detection (PCR, ELISA, and so on) and DNA detection (Southern blot, GC/MS, and so on), have the disadvantages of high costs, time‐consuming, complex operations, and destructive of the samples. Terahertz spectroscopy (THz) is a brand‐new radiation with many unique advantages. Most biological macromolecules have fingerprint characteristics in THz band from the current recognition. In this study, feasibility of identifying the transgenic cotton seeds from nontransgenic counterparts using THz spectroscopy method was investigated. The transgenic cotton seeds‐Lumianyan No.28 and nontransgenic cotton seeds‐Xinluzao No.51 were selected and the sample‐making methods were studied; then the refractive and absorption curves of samples were got and given a detailed discussion; finally, absorption index of transgenic and nontransgenic DNA was observed and discussed. The results showed there were small fluctuations in THz band, and refractive index of transgenic seeds was lower than nontransgenic ones and had obvious turning point at 1.4–2.0 THz region. There were significant peaks in 1.0–1.2 and 1.3–1.5 THz regions for the transgenic cotton seeds. Transgenic DNA had higher absorption index than nontransgenic DNA, and there were 3–4 peaks corresponding to the cotton seed samples in 1.0–1.6 THz region. These results showed cotton seeds samples can provide important bio‐information in THz band, and this study provided a basis for developing potential THz‐based gene detection technologies.

Effects of inter‐species chromosome substitution on cottonseed mineral and protein nutrition profiles

AbstractUpland cotton (Gossypium hirsutum L.) is the major species of cotton due to its high yield and good adaptability. With much less land area, pima cotton (G. barbadense L.) is also cultivated for its superior fibers. Existing research efforts have mainly focused on introgression of fiber quality traits from pima into upland cotton, with few on the seed mineral and protein contents. In this research, we used a multi‐parent advanced generation inter‐crossing (MAGIC) population that was derived from crosses between 18 pima cotton chromosome substitution lines and 3 Upland cultivars to understand the profile of the seed mineral and protein contents. We evaluated the contents of mineral and protein in the seeds of 21 parental and their 177 progenies. The profile patterns of these parameters were not always the same in the individual cottonseed samples. The contents of Ca, K, and B were different among both parental and progeny lines. In addition, the contents of Cu and Mn were also different (p ≤ .05) among the 21 parents. In contrast, there were four additional elements (Mg, Fe, Zn, and Ni) differing significantly in content among the progeny samples. These observations implied that chromosome substitution had impacts on the profile of the mineral nutrients in cottonseed. The data identifying the top five cotton lines with the highest and lowest contents of each element and protein provide a base for researchers and breeders to select better and/or preferred seed quality, in addition to the assurance of lint yield and quality, for further development.

Dual-template imprinted polymers for class-selective solid-phase extraction of seventeen triazine herbicides and metabolites in agro-products.

A novel dual-template molecularly imprinted polymer (DMIP) was prepared with atrazine and prometryn as the template and applied as a class-specific adsorbent for simultaneously selective solid-phase extraction of seventeen triazine herbicides and metabolites from complex matrices. For comparison, a non-imprinted polymer (NIP) and two single-template imprinted polymers (SMIPs) were also synthesized using the same procedure of DMIP, but in the absence of the template (NIP) or with one template (SMIP). Various parameters affecting the extraction performance of DMIP-SPE were investigated in detail. Under the optimum conditions, the enrichment efficiency, class-selectivity and reusability of DMIP-SPE were evaluated. Only DMIP-SPE possessed high affinity and good selective recognition ability for all the seventeen targets including chloro-, thiomethyl- and methoxy- triazines. Further, a DMIP-SPE-LC-MS/MS method was developed for simultaneously determining trace triazine herbicides and metabolites in maize, wheat and cottonseed samples. The method showed good linearity (r>0.9941) in the range of 10-200 μg kg-1, high sensitivity with low limits of detection of 0.5-8.8 μg kg-1, and satisfactory recoveries of 61.3-105.9% with relative standard deviations of 2.1-10.7%. These results highlighted the good application prospect of the multi/dual-template imprinting strategy in the high-throughput analysis of various concerned contaminants in agro-products.

Analysis of fatty acid composition in cottonseed by gas chromatography with on-line pyrolytic methylation

A method of on-line pyrolytic methylation-gas chromatography was developed for the analysis of fatty acid composition in cottonseed. Fatty acids in cottonseeds were converted to their corresponding fatty acid methyl esters in the presence of trimethylsulfonium hydroxide at 300℃. The major fatty acids were linoleic acid (C18:2), oleic acid (C18:1), palmitic acid (C16:0), stearic acid (C18:0), myristic acid (C14:0), palmitoleic acid (C16:1), arachidic acid (C20:0) and docosanoic acid (C22:0). The unsaturated fatty acid content varied from 66.30% to 72.54%, and linoleic acid content varied from 43.20% to 53.61%. The RSDs of the peak areas of the fatty acids were less than 10% (n=5). The fatty acid compositions in the cottonseed samples, obtained from different growing places and different edible oil samples were compared by statistical analysis. The results showed that fatty acid compositions in cottonseed samples from different regions were similar. The fatty acid composition in cottonseed samples was closest to that of corn oil, and the similarity varied from 0.960 to 0.992. The method is simple, rapid, accurate, and is suitable for the analysis of fatty acid composition in cottonseed.

Rapid determination of phytic acid content in cottonseed meal via near infrared spectroscopy

A near infrared calibration model with higher precision and better stability was constructed in the present study, using 280 cottonseed samples. The reference phytic acid contents were determined by high-performance ion chromatography. A combination of Savitzky–Golay smoothing, standard normal variate, and the first derivative was chosen as the spectral pre-treatment method. Monte Carlo uninformative variable elimination was proposed for spectral variable selection. The regression methods of partial least squares, least squares support vector machines, and weighted least squares support vector machines were developed for the calibration model. The optimal near infrared calibration model for phytic acid contents in the cottonseed meals was least squares support vector machines, with r2 = 0.97, RPD = 5.53, RMSECV = 0.06%, and RMSEP = 0.05%. This robust method can replace the traditional method of phytic acid determination in cottonseed meals.

Electrical properties of vegetable oils between 20 Hz and 2 MHz

Electrical properties (permittivity and conductivity) of vegetable oils were determined in the frequency range from 20 Hz to 2 MHz. Commercial samples of corn, sunflower, soybean, grapeseed, cottonseed, olive, canola and chia oils were measured at temperatures between 300 K and 343 K (stabilized within 0.1 K). The calibration uncertainty in the measuring system was below 1%.In all the measured samples the real part of the relative permittivity decreases with temperature, with a very good fit to a linear function; and it clearly depends on the oil source. The conductivity increases rapidly with temperature, fitting satisfactorily to an Arrhenius function. The values of the activation energy are between 0.34 eV (chia) and 0.46 eV (olive and soybean), and are consistent with previously reported values. These results are relevant for the application of electrical properties to the characterization of oils during transport and storage, and also to monitor the progress of the transesterification reaction.

Mineral Composition of Cottonseed is Affected by Fertilization Management Practices

Cottonseed and its products can be used as human food, animal feed, and industrial raw material. Chemical composition is one of the critical parameters to evaluate cottonseed’s quality and potential end use. Whereas there are reports on the improvement of cotton (Gossypium hirsutum L.) lint yield by poultry litter (PL) fertilization, there are no data about the impact of PL application on mineral composition of cottonseed. In this study, we collected seed samples in 2 yr from cotton fertilized with PL and chemical inorganic fertilizer (CIF) with or without winter wheat (Triticum aestivum L.) cover crop (CC) at the Mississippi Agricultural and Forest Experiment Station. Contents of 18 elements (Al, As, B, C, Ca, Cd, Cu, Fe, K, Mg, Mn, N, Na, Ni, P, Pb, S, and Zn) and ash in these cottonseed samples were determined by inductively coupled plasma‐based or dry combustion methods. Cover crop did not significantly impact the chemical composition of cottonseed. Compared to no fertilizer control, both CIF and PL altered the levels of Ca, Mg, Cu, Fe, Mg, Mn, P (possibly Na and K), and ash contents but not C, N, Zn, Ni, Cd, Pb, Al, S, B and As. The impact of subsurface band vs. broadcast application methods or fall vs. spring application timing on mineral composition was not obvious. Cottonseed K, Mg, and P contents were higher with PL fertilization but lower with CIF than those of the control cottonseed (no fertilizer). The data of the three elements were highly correlated (α < 0.01), indicating the three elements were co‐accumulated in cottonseed.

Persistence of Acephate and Cypermethrin on Cotton Leaves, Cottonseed, Lint and Soil

Following foliar applications of combination formulation (cypermethrin 5% + acephate 45% DF) at 850 and 1,700 g ha(-1), resulting in active application of acephate at 382.5 and 765 g a.i. ha(-1) whereas active application of cypermethrin at 42.5 and 85 g a.i. ha(-1), the average initial deposits of acephate on cotton leaves were found to be 13.45 and 27.73 mg kg(-1), at single and double the doses of application, respectively. Residues of acephate declined below detectable level of 0.02 mg kg(-1) after 15 days of applications at application rates with t ((1/2)) values of 1.56 and 0.68 days, respectively. Similarly, the average initial deposits of cypermethrin were found to be 22.31 and 32.45 mg kg(-1), respectively. Cypermethrin residues reached below its detectable level of 0.02 mg kg(-1) after 21 days of its application at both the dosages of application. The half-life values for cypermethrin were observed to be 0.71 and 0.69 days, corresponding to single and double the dose of application, respectively. Interestingly, none of the samples of cottonseed, lint and soil showed presence of acephate or cypermethrin at the detection limit of 0.02 mg kg(-1) at first pick of the harvest time of the crop.

Thermodynamic properties and moisture adsorption isotherms of cottonseed protein isolate and different forms of cottonseed samples

Moisture adsorption isotherms of fuzzy cottonseed, black cottonseed, whole cottonseed kernel, blended cottonseed kernel and its protein isolate were obtained using gravimetric static method at 15, 25, 35 and 45 °C. GAB, Halsey and Harkins–Jura equations gave the best fit to experimental data among 14 well-known equations tested. M 0 values of samples calculated by G.A.B. and B.E.T. equations decreased with increasing temperature. The moisture adsorption isotherms obtained were type II sigmoidal. Thermodynamic properties such as differential enthalpy and entropy were determined from moisture adsorption data, using Clausius–Clapeyron equation. The experimental data showed that enthalpy–entropy compensation theory was applicable for the moisture adsorption behaviours of cottonseed samples and the adsorption process of samples was enthalpy-controlled.

Natural occurrence of type B trichothecenes in formula feeds and feedstuffs in Japan

The natural occurrence of type B trichothecenes (deoxynivalenol (DON), 3-acetyldeoxynivalenol(3-ADON), 15-acetyldeoxynivalenol (15-ADON), nivalenol (NIV) and fusarenone-X (F-X)) was investigated in formula feeds and feedstuffs. Twenty-one formula feed samples and 44 feedstuff samples (maize, milo, barley, wheat, rye, wheat bran, soybean meal, rapeseed meal, and cottonseed) were collected from the Japanese Feed Industry. These samples were analyzed by gas chromatography after purification with a multifunctional cleanup (MFC) column and trimethyl silyl derivatization. DON was detected in formula feed, cereals and bran samples. The concentrations in positive samples were 16~190 μg/kg in formula feeds and 14~2,200 μg/kg in cereals and wheat bran. 15-ADON was detected in formula feed, maize, wheat and wheat bran samples at concentrations of 10~94 μg/kg in positive samples. NIV was detected in the samples of formula feed, milo, barley, rye, wheat and wheat bran samples at concentrations of 26~140 μg/kg in positie samples. 3-ADON and F-X were not detected in any sample. None of the samples of cottonseed, soybean meal and rapeseed meal contained these trichothecenes.

Mites associated with stored seed cotton and related products in Greece

Samples were taken during a 2-year period (Sept. 1998 to Sept. 2000) from 17 ginning mills, located in the main cotton production regions in Greece. The material was examined in order to determine the presence and relative abundance of mites in stored seed cotton and its products: cotton fiber, cottonseed and cotton gin trash. Twenty-two mite taxa were found, with the predominance of mite species on each type of stored commodity differing significantly. Fifteen taxa were recorded in seed cotton, where the most abundant species wereTyrophagus putrescentiae (Schrank) andTarsonemus waitei Banks. In contrast, only four species were found in cotton fiber, withT. putrescentiae being the dominant one. Nine taxa were recorded in the cottonseed samples, where the most abundant species was by farLepidoglyphus destructor (Schrank).Caloglyphus sp. was the most abundant species in cotton gin trash, where a total of 13 taxa were found. Most mites were found in gin trash, followed by cottonseed and seed cotton; very few mites were detected in cotton fiber.

Naturally occurring toxins in feedstuffs: Center for Veterinary Medicine Perspective

The objectives of this review are to provide 1) information on the FDA Feed Contaminants Program, 2) the legal history of aflatoxins and their current action levels, 3) a report on the levels of aflatoxins, fumonisins, vomitoxin, ochratoxin A, and zearalenone in domestic and import surveillance samples of feed during fiscal years 1989 through 1992, and 4) information on naturally occurring toxins encountered recently by the Center for Veterinary Medicine. Ten of 644 (1.6%) domestic corn samples and 7 of 106 (6.6%) domestic cottonseed samples contained aflatoxins at levels > 300 ppb. The mean fumonisin level in the 1990 survey of 85 corn screening samples was 12.1 ppm, and the values ranged from 2.6 to 32 ppm. The mean vomitoxin levels in the 1991 survey of 207 winter wheat samples and 206 spring wheat samples was 2.4 and .9 ppm, respectively. Ochratoxin A was not detected in 168 samples. Zearalenone was detected at levels > .15 ppm in only 1 of 161 samples. Cottonseed containing 13,000 ppm gossypol was recently implicated in the deaths of dairy cows. Crambe meal and canola meal are sanctioned for use in feed with certain restrictions, including the levels of glucosinolates. The FDA is continuing its surveillance and will strive to provide guidance on the increasing number of naturally occurring toxins.

Liquid Chromatographic Determination of Unbound and Acetone-Soluble Bound Gossypol in Cottonseed Meals and Mixed Feeds

Abstract A liquid chromatographic method has been developed for the determination of unbound and acetone- soluble bound gossypol in cottonseed meals and mixed feeds at levels of 0.5 ppm. The method involves extraction with aqueous acetone in the presence of ascorbic acid, hydrolysis of the "soluble bound" forms with hydrochloric acid, partitioning into chloroform, and chromatographic separation on a 10 µm C18 column by step gradient elution using a methanol-water mobile phase acidified with phosphoric acid. With minor modifications, the method permitted discriminate determination of unbound gossypol and acetone-soluble hydrophilic and lipophilic forms of bound gossypol. The gossypol peak was characterized by on-line spectral scanning and absorbance rationing. Overall relative standard deviation was 6.7% and overall recovery was 98.1 ± 3.3%. When the method was applied to several cottonseed meal samples, results were inconsistent with those obtained by the official American Oil Chemists' Society method for "free" gossypol determination.

Microwave heating to prevent deterioration of cottonseed during storage

AbstractFuzzy cottonseed samples of 14.5% moisture and <1.0% free fatty acids (FFA) contents heated in a conventional, home‐style microwave oven at 700W and 2450 MHz for intervals up to 2.0 min. The 2.0‐min treatment reduced the moisture content to 13.1%. Examination of the seed immediately after microwave heating (MWH) indicated no differences in the proteins or in the quality or quantity of the cotton linters as compared with unheated seed. Neither the oil content of the seed nor the quality of the oil were affected by the microwave treatment. After nine weeks of storage at 50°C, the unheated seed had a FFA content of >3.0% while the FFA content of the 2.0‐min microwave‐heated seed remained <1.0%. During this storage period there was significant deterioration of the protein quality of the unheated seed. The 2.0‐min MWH treatment, however, maintained the integrity of the protein during storage.

Sample Collection and Sample Preparation Techniques for Aflatoxin Determination in Whole Cottonseed

Abstract The present paper describes a comparative study between sampling devices used In the official sampling plan for Arizona cottonseed and a device that provides a smaller sampling size. The official sample must be greater than 30 lbs from at least ten 3 lb probes/cottonseed lot, not exceeding 100 tons. This Is accomplished using a Probe-A-Vac pneumatic or corkscrew sampler with a 3 in. diameter X 50 In. probe. The alternative sampling device evaluated In this study uses a modified shop-vac wet-dry vacuum with a 0.75 in. diameter X 100 in. probe. Ten 1 lb probes were taken for a total sample size of 10 lbs. Aflatoxin concentrations in cottonseed samples taken using both sampling probes at adjacent points throughout the lot were determined with an AOAC thin-layer chromatographic method (26.052-26.059, 14th Ed., 980.20AH, 15th Ed.). Mean total aflatoxin concentrations for Probe-AVac vs shop-vac samples from 39 lots (1987-1988 crop year) and 21 lots (1988-1989 crop year) were 76.6 vs 68.5 and 39.5 vs 30.7 µg/kg, respectively. Long staple cottonseed was sampled using a long staple trier (LS Trier), an alternative for which may be the shop-vac system. Mean total aflatoxin concentrations for LS Trier vs shop-vac for 7 lots (1988-1989 crop year) were 9.4 vs 5.1, µg/kg respectively. Also, an ultracentrlfugal mill has proven to be highly versatile for both denuding and grinding cottonseed to be tested under both laboratory and nonlaboratory situations.

Investigation by fractional crystallization of classes of compounds formed during frying of vegetable oils

In an effort to standardize a rapid and reliable method for the characterization of thermally abused vegetable oils, the technique of fractional crystallization was applied to heated samples of cottonseed and corn oil. Using this method an insoluble fraction enriched mainly in polar compounds, which form during the heating process, was obtained. These compounds, mostly of high molecular weight, are responsible for the increase in viscosity of the oil and are retained in a gas chromatographic column used for fatty acid methyl ester analysis. It was found that the above insoluble fraction formed when heated samples contained 25% polar constituents, a value which is widely accepted as the upper limit for use of heated vegetable oils. It is proposed that the technique of fractional crystallization can be used as a method for rapid quality assessment of frying oils such as non-hydrogenated vegetable oils.