Multi-scale characterization and mechanistic comparison of acid–alkali pretreatment during cell wall deconstruction of Achnatherum splendens

Zhennan He , Guolin Yang , Siyi Wang , Yuanyuan Jing , Fengqin Gao

Bioresources and Bioprocessing ›› 2026, Vol. 13 ›› Issue (1) : 119

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Bioresources and Bioprocessing ›› 2026, Vol. 13 ›› Issue (1) :119 DOI: 10.1186/s40643-026-01097-2
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Multi-scale characterization and mechanistic comparison of acid–alkali pretreatment during cell wall deconstruction of Achnatherum splendens
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Abstract

Achnatherum splendens was used as a high-lignin herbaceous feedstock to compare the effects of dilute sulfuric acid and sodium hydroxide pretreatments on component degradation and cell wall structure. Chemical composition analysis, X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), and scanning electron microscopy (SEM) were used for multi-scale characterization. The results showed that dilute sulfuric acid pretreatment mainly promoted hemicellulose degradation, with a hemicellulose degradation rate of 79.2% under 1.5% H2SO4, while lignin dissolution remained limited at 20.5%. In contrast, NaOH pretreatment showed stronger lignin removal and fiber separation, with lignin dissolution increasing to 44.8% at 4% NaOH. Both pretreatments increased cellulose crystallinity from 47.0% to between 53.4 and 60.8%, whereas crystallite size showed no significant change, indicating that the crystalline cellulose domains were largely preserved. FTIR results showed spectral inconsistencies after acid treatment, including increased absorbance at 1510 cm−1 and limited reduction at 1730 cm−1, which may be associated with pseudo-lignin-related interference. SEM observations showed that acid treatment generated pores and cracks, whereas alkali treatment resulted in more obvious fiber bundle separation and surface cleaning. These results indicate that acid and alkali pretreatments have complementary effects on the deconstruction of Achnatherum splendens. The findings provide structural-level evidence for pretreatment selection and optimization of high-lignin energy grasses.

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Achnatherum splendens / Dilute sulfuric acid / Sodium hydroxide / Cellulose crystallinity / Lignocellulose

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Zhennan He, Guolin Yang, Siyi Wang, Yuanyuan Jing, Fengqin Gao. Multi-scale characterization and mechanistic comparison of acid–alkali pretreatment during cell wall deconstruction of Achnatherum splendens. Bioresources and Bioprocessing, 2026, 13 (1) : 119 DOI:10.1186/s40643-026-01097-2

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References

[1]

Behera S, Arora R, Nandhagopal N, et al. . Importance of chemical pretreatment for bioconversion of lignocellulosic biomass. Renew Sust Energ Rev, 2014, 36: 91-106

[2]

Chen N, Jiang K, Zhao M, Zhang C, Jin Y, Wu W. Pretreatment process of lignocellulosic biomass: a review of pseudo-lignin formation. Biomass Bioenergy, 2024, 188 107339

[3]

Cui L, Wei X, Li J et al (2017) Structure and saccharification of sugarcane bagasse pretreated with acid coupled alkaline. In: International symposium on mechanical engineering and material science (ISMEMS 2017). Atlantis Press, pp 104–107

[4]

DeMartini JD, Pattathil S, Miller JS, et al. . Investigating plant cell wall components that affect biomass recalcitrance in poplar and switchgrass. Energy Environ Sci, 2013, 6(3): 898-909

[5]

Dickens B, Mauer FA, Brown WE. A refinement of the crystal structure of Na2CO3· H2O. J Res Natl Bur Stand Sect A Phys Chem, 1970, 74(3): 319

[6]

Do TA, Nguyen VQ, Nguyen TMC, et al. . A one-step chemical treatment to directly isolate microcrystalline cellulose from lignocellulose source. Bioresour Bioprocess, 2025, 12189

[7]

Gao FQ, Jing YY, De Y, et al. . Effects of dilute sulfuric acid pretreatment on chemical composition and structural characteristics of lignocellulose in hybrid Pennisetum. Sci Agric Sin, 2020, 53214516-4526

[8]

Gao FQ, Tao Y, Wu HX, et al. . Effect of dilute alkali pretreatment on lignocellulose degradation of hybrid Pennisetum. Chin J Grassl, 2020, 42(1): 58-67

[9]

Gao F, Wang H, Jiang H, et al. . Evaluation of lignocellulose degradation and ethanol production via dilute acid and alkali pretreatment of hybrid Pennisetum. BioResources, 2022, 17(3): 4517

[10]

Harabor A, Rotaru P, Harabor NA. Two phases in a commercial anhydrous sodium carbonate by air contact. Physics AUC, 2013, 23: 79-88

[11]

Hasan MH, Hossain S, Rahman ML, et al. . Effect of hydrolysis agitation and suspension drying temperature on the synthesis of crystalline cellulose from jute fiber. Carbohydr Polym Technol Appl, 2025, 10100769

[12]

Hendriks A, Zeeman G. Pretreatments to enhance the digestibility of lignocellulosic biomass. Bioresour Technol, 2009, 100(1): 10-18

[13]

Himmel ME, Ding SY, Johnson DK, et al. . Biomass recalcitrance: engineering plants and enzymes for biofuels production. Science, 2007, 315(5813): 804-807

[14]

Hossen MT, Kundu CK, Pranto BMRR, et al. . Synthesis, characterization, and cytotoxicity studies of nanocellulose extracted from okra (Abelmoschus esculentus) fiber. Heliyon. 2024

[15]

Hu F, Jung S, Ragauskas A. Pseudo-lignin formation and its impact on enzymatic hydrolysis. Bioresour Technol, 2012, 1177-12

[16]

Ji Z (2016) Study on the deconstruction of plant cell wall during dilute acid and alkali pretreatment. Doctoral Dissertation, Beijing Forestry University, Beijing

[17]

Kapoor M, Raj T, Vijayaraj M, et al. . Structural features of dilute acid, steam exploded, and alkali pretreated mustard stalk and their impact on enzymatic hydrolysis. Carbohydr Polym, 2015, 124: 265-273

[18]

Kar A, Saikia D, Pandiarajan N. Characterization of alkali-treated cellulosic fibers derived from Calamus tenuis canes as a potential reinforcement for polymer composites. Biomass Convers Biorefin, 2025, 15(5): 7881-7899

[19]

Kaur J, Taggar MS, Kalia A, et al. . Assessment of the chemical pre-treatment methods for the delignification of sugarcane bagasse. Environ Technol, 2025, 46(17): 3363-3373

[20]

Kim TH, Lee YY. Pretreatment of corn stover by soaking in aqueous ammonia at moderate temperatures. Appl Biochem Biotechnol, 2007, 137(1): 81-92

[21]

Kruer-Zerhusen N, Cantero-Tubilla B, Wilson DB. Characterization of cellulose crystallinity after enzymatic treatment using Fourier transform infrared spectroscopy (FTIR). Cellulose, 2018, 25(1): 37-48

[22]

Kululo WW, Habtu NG, Abera MK, et al. . Advances in various pretreatment strategies of lignocellulosic substrates for the production of bioethanol: a comprehensive review. Discov Appl Sci, 2025, 7(5): 476

[23]

Li H, Pu Y, Kumar R, et al. . Investigation of lignin deposition on cellulose during hydrothermal pretreatment, its effect on cellulose hydrolysis, and underlying mechanisms. Biotechnol Bioeng, 2014, 1113485-492

[24]

Li Q, Li X, Jiang Y, et al. . Analysis of degradation products and structural characterization of giant reed and Chinese silvergrass pretreated by 60Co-γ irradiation. Ind Crop Prod, 2016, 83: 307-315

[25]

Miao LP, Huo L, Xu L, et al. . Study on the enhanced enzymatic hydrolysis of wheat straw by alkaline hydrogen peroxide pretreatment. J Cellul Sci Technol, 2018, 26(4): 45-51

[26]

Nair LG, Verma P. Harnessing carbon potential of lignocellulosic biomass: advances in pretreatments, applications, and the transformative role of machine learning in biorefineries. Bioresour Bioprocess, 2025, 12(1): 97

[27]

Ni TR (2010) Study on the pretreatment of Achnatherum splendens for fuel ethanol conversion. Master's Thesis, Lanzhou Jiaotong University, Lanzhou

[28]

Palmqvist E, Hahn-Hägerdal B. Fermentation of lignocellulosic hydrolysates. II: inhibitors and mechanisms of inhibition. Bioresour Technol, 2000, 74125-33

[29]

Pari P, Eshtiaghi N, Othman M, et al. . A comparative assessment and economic implications of physical, chemical, and enzymatic treatments of lignocellulosic waste. Bioresources and Bioprocessing, 2025, 12(1): 115

[30]

Premjet D, Premjet S. Enhanced sugar and bioethanol production from broom grass via NaOH-autoclave pretreatment. Polymers (Basel), 2025, 173266

[31]

Ren J, Tao L, Ni TR (2015) Effects of liquid-to-solid ratio and reaction time on dilute sulfuric acid pretreatment of Achnatherum splendens. pp 2133–2136

[32]

Sannigrahi P, Kim DH, Jung S, et al. . Pseudo-lignin and pretreatment chemistry. Energy Environ Sci, 2011, 441306-1310

[33]

Scherrer P. Bestimmung der Grösse und der inneren Struktur von Kolloiteilchen mittels Röntgenstrahlen. NachrEn Ges Wiss Zu Gottingen Math-Phys KlE, 1918, 1: 96-100

[34]

Segal L, Creely JJ, Martin AEJr, et al. . An empirical method for estimating the degree of crystallinity of native cellulose using the X-ray diffractometer. Text Res J, 1959, 29(10): 786-794

[35]

Sethi N, Luhach N, Kirrolia AS, et al. . Physicochemical characterization of rice straw before and after alkali-assist photocatalytic pretreatment: a comparative analysis. Environ Sci Pollut Res, 2025, 32(52): 29581-29591

[36]

Sheng Y, Lam SS, Wu Y, Ge S, Wu J, Cai L, Huang Z, Le QV, Sonne C, Xia C. Enzymatic conversion of pretreated lignocellulosic biomass: a review on influence of structural changes of lignin. Bioresour Technol, 2021, 324 124631

[37]

Shi R, Zhang Z, Zhang J, et al. . A comparative study on enhanced enzymatic hydrolysis of diverse herbaceous and woody wastes by promising dilute acid and alkaline pretreatments. Bioresour Bioprocess, 2025, 12(1): 36

[38]

Silverstein RA, Chen Y, Sharma-Shivappa RR, et al. . A comparison of chemical pretreatment methods for improving saccharification of cotton stalks. Bioresour Technol, 2007, 98163000-3011

[39]

Tao L et al (2013) Effects of liquid-to-solid ratio and reaction temperature on NaOH pretreatment of Achnatherum splendens. pp 3545–3548

[40]

Van Soest PJ, Robertson JB, Lewis BA. Methods for dietary fiber, neutral detergent fiber, and nonstarch polysaccharides in relation to animal nutrition. J Dairy Sci, 1991, 74(10): 3583-3597

[41]

Wakudkar H, Mandal S, Rani A, et al. . Experimental investigations on valorization of corncob residues for synthesis of crystalline cellulose. Biomass Convers Biorefin, 2025, 15(22): 29273-29281

[42]

Wang K, Guo H, You S, et al. . Interpretive analysis of the relationship between pseudolignin structure and enzymatic hydrolysis. Ind Crop Prod, 2024, 214 118519

[43]

Xu J, Cheng JJ. Pretreatment of switchgrass for sugar production with the combination of sodium hydroxide and lime. Bioresour Technol, 2011, 102(4): 3861-3868

[44]

Zhang C, Cheng L, Zhou X, et al. . Comparative evaluation of dilute acid, alkaline, and deep eutectic solvent pretreatments on enzymatic hydrolysis of sunflower stalk bark. Appl Biochem Biotechnol, 2025, 197(9): 5774-5789

[45]

Zhang H, Jia X, Ding K, Liang X, He Y, Guo X, Zhou L, Han L, Xiao W. Optimizing lignocellulose conversion: a comparative study of alkali-assisted ball milling pretreatment of cotton stalk and corn stover. J Biotechnol. 2025

[46]

Zheng MX, Li LQ, Zheng MY, et al. . Effect of alkali treatment on the cellulose structure of corn stover. Environ Sci Technol, 2012, 35(6): 27-31

Funding

earmarked fund for Inner Mongolia Agriculture and Animal Husbandry Research System(IMAHRS-9)

2023 National Center of Pratacultural Technology Innovation Major Innovation Platform Construction Project(CCPTZX2023B07)

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