【特约专题】

蛋白分离纯化材料的研究进展

赵雅琪，张新悦，黄倩，孙雪，钱俊莉，董林毅^*

(天津医科大学 药学院，天津  300070) 

摘要：蛋白质分离纯化是生物化学、生物技术及生物制药等领域中的关键环节，其效率和质量直接影响后续应用。随着生物技术的快速发展，新型材料的不断涌现为蛋白质纯化提供了更高效、更特异的方法，推动了该领域的革新。首先回顾了传统的蛋白质分离技术，如盐析沉淀、萃取、电泳、透析和色谱等，在过去几十年中得到了广泛应用和改进。这些方法虽然成熟且稳定，但仍存在灵敏度低、分辨率较差、操作繁琐等问题。接着，论述了新型蛋白质纯化材料及应用实例。例如，纳米材料（如磁性纳米颗粒、碳纳米管、碳量子点）具有高比表面积和可功能化特性，可提高吸附容量和选择性；高分子聚合物（如分子印迹聚合物、功能化聚合物材料）通过结构可设计性，进一步优化了蛋白纯化的效率和特异性；生物材料（如多糖、核酸适配体）能实现高度特异性的靶向结合，减少非特异性吸附。此外，还对未来蛋白质纯化技术的发展趋势进行展望，将趋向于智能化、自动化和绿色可持续化，旨在为该领域的进一步发展和创新提供参考。

关键词：蛋白质；分离纯化；传统技术；高分子聚合物；纳米材料；生物材料

中图分类号：O65         文献标识码：A          文章编号：0258-3283（2025）07-0001-09

DOI：10.13822/j.cnki.hxsj.2025.0064

Research Progress on Protein Separation and Purification Materials  ZHAO Ya-qi, ZHANG Xin-yue, HUANG Qian, SUN Xue, QIAN Jun-li, DONG Lin-yi^* ( School of Pharmacy, Tianjin Medical University, Tianjin 300070, China)

Abstract：Protein separation purification remains a fundamental process in disciplines including biochemistry, biotechnology, and biopharmaceuticals, with its efficiency and quality directly impacting downstream applications. With the rapid advancement of biotechnology, the ongoing development of new materials has enabled more efficient and specific methods for protein purification, driving innovation in this field. This review first summarizes traditional protein separation techniques, including salting-out precipitation, extraction, electrophoresis, dialysis, and chromatography, which have been widely applied and improved in the past few decades. Despite their maturity and reliability, these methods still face challenges such as low sensitivity, poor resolution, and cumbersome operation. Next, the review elaborates on novel protein purification materials along with their application examples. For instance, nanomaterials (e.g., magnetic nanoparticles, carbon nanotubes, carbon quantum dots) exhibit high specific surface area and functionalization capability, which can significantly enhance adsorption capacity and selectivity. Polymeric materials (e.g., molecularly imprinted polymers, functionalized polymer materials) optimize purification efficiency and specificity through their designable structures. Additionally, biomaterials (e.g., polysaccharides, nucleic acid aptamers) enable highly specific target binding while minimizing nonspecific adsorption. Additionally, it provides forword-looking insights into their future development trends, which are anticipated to evolve toward intelligent systems, full automation, and green sustainable solutions. These advancements aim to provide valuable references for further progress and innovation in the field.

Key words: protein; separation and purification; traditional techniques; polymer; nanomaterials; biomaterials

硫磺：从传统到新兴领域的多元应用

田俊，高文超^*

(太原理工大学 化学与化工学院，山西 太原  030024)

摘要：硫磺作为一种自然界中广泛存在的非金属单质，在人类文明的演进历程中占据着不可替代的地位。自远古时代起，硫磺凭借其独特的化学性质很早就融入人类的生产生活，被广泛应用于医药、香料及宗教仪式等场景。自19世纪以来，硫磺作为石油和天然气工业的副产品被大量生产，从而推动硫磺的应用领域持续拓展，从传统的化工、农业等领域，延伸至现代新兴科技范畴，见证了无数技术革新与社会变迁。当前，传统行业的稳定增长和新兴产业的爆发式发展更加推动了硫磺需求的攀升。当然，随着环保和可持续发展的需求增加，硫磺的资源化利用正朝着绿色化转型，特别是近几十年以来，硫磺的储能特性被逐步开发后，使其在新材料、新能源和生物医药等前沿科技领域，展现出巨大的应用与发展潜力。全面剖析硫磺的结构特点、产能来源、基本性质，并着重从化学本质的角度系统梳理硫磺在传统行业与新兴产业的多元应用及发展前景，为硫磺的深入研究和发展应用提供思路与方向。

关键词：硫磺；含硫材料；新能源；含硫药物；逆硫化反应

中图分类号：O69            文献标识码：A             文章编号：0258-3283（2025）07-0010-08

DOI：10.13822/j.cnki.hxsj.2025.0082

Sulfur: Diverse Applications from Conventional to Emerging Fields  TIAN Jun, GAO Wen-chao^* ( School of Chemistry and Chemical Engineering, Taiyuan University of Technology, Taiyuan 030024, China) 

Abstract：As a non-metallic element widely present in nature, sulfur occupies an irreplaceable position in the evolution of human civilization. Since ancient times, due to its unique chemical properties, sulfur has been integrated into human production and daily life at an early stage, and has been widely used in scenarios such as medicine, spices, and religious ceremonies. Since the 19th century, sulfur has been mass-produced as a by-product of the petroleum and natural gas industries, which has continuously expanded the application fields of sulfur. From traditional fields such as chemical engineering and agriculture, it has extended to the realm of modern emerging technologies, witnessing countless technological innovations and social changes. Currently, the stable growth of traditional industries and the explosive development of emerging industries have further driven the increase in the demand for sulfur. Of course, with the increasing demand for environmental protection and sustainable development, the resource-based utilization of sulfur is undergoing a green transformation. Especially in recent decades, after the energy storage characteristics of sulfur have been gradually developed, it has demonstrated great application and development potential in cutting-edge technological fields such as new materials, new energy, and biomedicine. This review aims to comprehensively analyze the structural characteristics, production capacity sources, and basic properties of sulfur, and focuses on systematically sorting out the diversified applications and development prospects of sulfur in traditional industries and emerging industries from the perspective of its chemical essence, providing ideas and directions for in-depth research, development, and application of sulfur.

Key words：sulfur; sulfur-containing materials; new energy technology; sulfur-containing drugs; inverse vulcanization 

近红外光谱技术在复杂组分样品中的应用进展

丁超民^,2，李轲^*1，刘帆¹，张鑫^1,2，李琪¹，张正东^*1

(1. 中国计量科学研究院 环境计量中心，北京  100029；2. 西南石油大学 化学化工学院，四川 成都  610500)

摘要：近红外光谱（NIR）技术作为一种无损、快速、非侵入性的分析手段，在快速检测、在线分析以及实时监测等方面拥有巨大的应用潜力。化学计量学的发展和应用有效克服了NIR光谱维度较高和复杂背景干扰的问题，而近年来深度学习的发展进一步突破了传统建模方法的局限性，使得NIR技术在复杂组分样品中的定量分析和定性识别能力得到了显著提升。深度学习通过筛选和提取关键光谱信息，显著提升了模型对微弱信号和复杂光谱的解析能力，从而拓宽了NIR技术在复杂样品分析中的应用空间。简要介绍了近红外光谱技术的原理，重点综述了NIR光谱结合化学计量学在石油化工、农业、环境科学、食品科学及药物分析多领域的应用进展，如原油理化性质分析、农作物成分评估及环境污染物监测等方向。通过建立高性能的化学计量学模型，NIR技术可成功实现待测物质的理化性质测定及产品质量控制等方面的应用。综上，对近红外光谱技术在多领域中的应用现状进行了系统性阐述，并对各领域的发展应用进行了总结及展望。

关键词：近红外光谱；化学计量学；石油化工；农业；食品科学；环境科学

中图分类号：O657.33        文献标识码：A           文章编号：0258-3283（2025）07-0018-10

DOI：10.13822/j.cnki.hxsj.2025.0052

Advancements in the Application of Near-Infrared Spectroscopy in Complex Compositional Samples 

DING Chao-min^1,2, LI Ke^*1 ,LIU Fan¹, ZHANG Xin^1,2, LI Qi¹, ZHANG Zheng-dong^*1

(1. Center for Environmental Metrology, National Institute of Metrology, Beijing 100029, China; 2. College of Chemistry and Chemical Engineering, Southwest Petroleum University, Chengdu 610500, China) 

Abstract：Near-infrared (NIR) spectroscopy, as a non-destructive, rapid, and non-invasive analytical technique, holds significant potential for applications in rapid detection, online analysis, and real-time monitoring. The development and application of chemometrics have effectively overcome the challenges posed by the high dimensionality of NIR spectra and complex background interferences. In recent years, the advancement of deep learning has further broken through the limitations of traditional modeling methods, significantly enhancing the quantitative analysis and qualitative identification capabilities of NIR technology in complex sample components. By selecting and extracting key spectral information, deep learning has greatly improved the model’s ability to analyze weak signals and complex spectra, thus expanding the application potential of NIR technology in complex sample analysis. Provides a concise overview of the principles of NIR spectroscopy, with a particular focus on the application advancements of NIR spectroscopy combined with chemometrics across various fields such as petrochemical, agriculture, environmental science, and food science. Notable applications include the analysis of the physicochemical properties of crude oil, evaluation of crop composition, and monitoring of environmental pollutants. By establishing high-performance chemometric models, NIR technology has successfully facilitated applications in determining the physicochemical properties of substances under analysis and ensuring product quality control. In conclusion, this paper systematically discusses the current state of NIR spectroscopy applications across multiple fields and offers a summary and outlook on future developments in these areas.

Key words：Near-Infrared spectroscopy; chemometrics; petrochemicals; agriculture; food science; environmental science

【功能材料】

负载Ni-Sn的MCM-22分子筛催化正辛烷脱氢裂解合成低碳烯烃

郭成雄，吴桂英，金放^*，朱圣东

(武汉工程大学  化工与制药学院，绿色化工过程教育部重点实验室，新型反应器与绿色化学工艺湖北省重点实验室，湖北 武汉  430205)

摘要：与传统的热裂解和催化裂解工艺相比，结合了烷烃脱氢和酸催化裂解两种活性位的脱氢裂解工艺可以提高石脑油裂解低碳烯烃的产率并降低能耗。为了研究设计新型石脑油脱氢裂解双功能催化剂中脱氢活性位和裂解活性位的协同效应，依据MWW分子筛酸性可调和富含羟基结构的特点，在MCM-22分子筛上通过原子原位移植引入Sn作为路易斯酸脱氢位点，采用沉积沉淀法引入Ni作为金属脱氢活性位，对分子筛的质子酸酸位点与引入Ni和Sn的脱氢活性位点进行了优化组合。引入的Ni颗粒（NPs）被SnO_x捕捉形成双金属镶嵌结构增强了路易斯酸强度，这种活性位点之间的协同作用促进了正辛烷脱氢裂解反应，提高了丙烯和乙烯的收率，并实现了对丙烯/乙烯（P/E）比例的控制。结果表明采用原子原位移植法负载Sn，SnCl₄会与分子筛骨架中的羟基发生脱氯化氢反应形成SnO_x物种，表现出明显的路易斯酸性。沉积-沉淀（DP）法负载的Ni纳米粒子可以被SnO_x电荷捕捉进一步增强路易斯酸强度，提高正辛烷转化率、低碳烯烃收率和P/E比。此外SnO_x物种在高温反应过程中从分子筛骨架析出为SnO₂并包裹Ni纳米颗粒形成核壳结构。这种结构显著减少了脱氢裂解过程中的积炭，提高了催化剂的稳定性。

关键词：脱氢；裂解；烷烃；Ni-Sn；路易斯酸；质子酸

中国分类号：O643.36       文献标识码：A         文章编号：0258-3283（2025）07-0028-07

DOI：10.13822/j.cnki.hxsj.2025.0070

Synthesis of Low-carbon Olefins by Dehydrocracking of N-octane Catalyzed with Ni-Sn-loaded MCM-22 Zeolite GUO Cheng-xiong, WU Gui-ying, JIN Fang^* (School of Chemical Engineering and Pharmacy, Wuhan Institute of Technology, Wuhan, Hubei，Key Laboratory for Green Chemical Process of Ministry of Education, Hubei，Novel Reactor & Green Chemical Technology Key Laboratory, 430205, China)

Abstract: Compared with the traditional thermal cracking and catalytic cracking processes, the dehydrogenation cracking process that integrates the two types of active sites for alkane dehydrogenation and acid-catalyzed cracking can enhance the yield of light olefins from naphtha cracking and reduce the energy consumption. In order to study and design the synergistic effect between the dehydrogenation active sites and the cracking active sites in a novel bifunctional catalyst for naphtha dehydrogenation cracking, based on the characteristics of the adjustable acidity and the hydroxyl-rich structure of MWW zeolites, Sn was introduced as a Lewis acid dehydrogenation site in the MCM-22 zeolite by the atom-planting method, and Ni was introduced as a metallic dehydrogenation active site by the deposition-precipitation method. An optimized combination was made for the proton acidic sites of the zeolite and the dehydrogenation active sites with the introduced Ni and Sn. The introduced Ni particles (NPs) were captured by SnO_x to form a bimetallic mosaic structure to enhance the Lewis acid strength and this synergistic interaction between the active sites facilitated the dehydrocracking reaction of n-octane, which increased the yields of propylene and ethylene, and realized the control of propylene/ethylene (P/E) ratio. The results indicate that Sn is loaded by the atom-planting method, SnCl₄ undergoes the dehydrochlorination reaction with the hydroxyl groups in the zeolite framework to form SnO_x species, which exhibit distinct Lewis acidity. The Ni nanoparticles loaded by the deposition-precipitation (DP) method can be captured by the charges of SnO_x, thereby further enhancing the Lewis acidity, which improves the n-octane conversion, yield of light olefins, and P/E ratio. In addition, SnOₓ species precipitates from the zeolite framework as SnO₂ during the high-temperature reaction and anchors the Ni NPs to form a core-shell structure. This structure significantly reduces the coke deposition and improves the stability of the catalyst.

Key words：dehydrogenation; cracking; alkane; Ni-Sn; Lewis acid; Brønsted acid

Cu₂O@CN_x材料的制备及光催化降解四环素应用研究

伍艺菲，胡杨，王思萍，付婉婷，吕春欣^*

（嘉兴大学 生物与化学工程学院，浙江 嘉兴  314001）

摘要：通过液相还原法成功制备了Cu₂O和氮掺杂材料（CN_x）的系列复合光催化材料Cu₂O@CN_x。采用FT-IR、XRD、SEM、HRTEM、XPS等多种表征手段对材料的结构、形貌和化学组成进行了全面分析。以四环素（TC）为模型污染物，在氙灯光源模拟可见光条件下，系统地考察了四环素降解反应的几个主要影响因素。实验结果表明，在模拟可见光300 W、四环素浓度20 mg/L、催化剂使用量30 mg、溶液pH 6的条件下，Cu₂O@CN_x-50作为催化剂，120 min后可以使100 mL的四环素降解率达到92%。由此可见，该催化剂在可见光催化领域表现出优异的催化性能。进一步研究了共存阴离子对催化体系的影响，发现NO₃^-对降解效率影响不大，SO₄^2-浓度低时对催化效果基本无影响，当浓度升高到10 mmol/L时，对四环素的降解起抑制作用。但CO₃²⁻因自由基捕获作用对四环素的降解影响显著，当浓度为5～10 mmol/L时可使降解率下降65%。自由基捕获实验证明了光生空穴(h⁺)与超氧自由基(·O₂⁻)在四环素降解中起主要作用。最后对Cu₂O@CN_x-50的稳定性进行了研究，重复使用4次后，TC的降解率有所下降。为开发高效稳定的可见光催化材料提供了新的思路，在环境污染物治理领域具有潜在的应用前景。

关键词：Cu₂O@CN_x；光催化；四环素；降解；可见光

中图分类号：O61              文献标识码：A              文章编号：0258-3283（2025）07-0035-08

DOI：10.13822/j.cnki.hxsj.2025.0027

Preparation of Cu₂O@CN_x Material and Its Application in Photocatalytic Degradation of Tetracycline WU Yi-fei, HU Yang, WANG Si-ping, FU Wan-ting, LV Chun-xin^*(College of Biological and Chemical Engineering, Jiaxing University, Jiaxing, 314001, China)

Abstract: Cu₂O and nitrogen doped (CN_x) composite photocatalytic materials Cu₂O@CN_x was successfully prepared by liquid phase reduction method. The structure, morphology and chemical composition of the materials were analyzed by FT-IR, XRD, SEM, HRTEM and XPS. Using tetracycline (TC) as a model pollutant, the main influencing factors of tetracycline degradation reaction were systematically investigated under simulated visible light irradiation from a xenon lamp The experimental results demonstrate that under conditions of 300 W simulated visible light, 20 mg/L TC concentration, 30 mg catalyst dosage, and pH 6, the Cu₂O@CN_x-50 catalyst achieve a 92% degradation rate of 100 mL TC solution within 120 minutes. This indicates that the catalyst exhibits excellent photocatalytic performance in the visible light range. Further investigation into the influence of coexisting anions on the catalytic system reveals that NO₃⁻ has little effect on the degradation efficiency, while SO₄²⁻ shows negligible impact at low concentrations but inhibited TC degradation when the concentration increased to 10 mmol/L. Notably, CO₃²⁻ significantly affects TC degradation due to its radical scavenging effect, reducing the degradation rate by 65% at concentrations of 5～10 mmol/L. The free radical capture experiment demonstrated that photo generated holes (h⁺) and superoxide radicals (O₂⁻) play a major role in tetracycline degradation. Then, the stability of Cu₂O@CN_x-50 is studied. After repeated use for 4 times, the degradation rate of TC decreases, which may be because the crystal structure of the catalyst shows more carbon peaks after 4 cycles. This work provides a new idea for the development of efficient and stable visible light catalytic materials, and has potential application prospects in the field of environmental pollution control.

Key words：Cu₂O@CN_x; photocatalysis; tetracycline; degradation; visible light

【电化学与新能源】

葡萄糖辅助溶剂热法制备多孔LiFe_0.4Mn_0.6PO₄/C材料

刘樟斌^1,2，李济澜^*2

(1. 大连大学 环境与化学工程学院，辽宁 大连  116622；

2. 六盘水师范学院 化学与材料工程学院，贵州 六盘水  553004)

摘要：橄榄石型LiFePO₄材料因其高理论容量（170 mAh/g）、优异的热稳定性、环境友好和低成本等优点而成为目前动力电池主要正极材料。然而LiFePO₄较低的工作电压（3.4 V vs. Li⁺/Li）导致其能量密度不高，同样具有橄榄石型结构的LiMnPO₄的工作电压达到4.1 V，因而具有更高的能量密度，可是LiMnPO₄的循环稳定性差。铁掺杂的LiFe_0.4Mn_0.6PO₄/C正极材料结合了LiFePO₄和LiMnPO₄的优点，具有高能量密度、良好的循环稳定性和安全性等优势，因而成为当今正极材料研究的热点材料之一。然而，要实现其大规模商业化应用，仍需进一步提高LiFe_0.4Mn_0.6PO₄/C材料的倍率性能和循环寿命。为了解决这些问题，研究人员发现构建多孔结构和碳包覆是最有效的方法之一。为此，采用葡萄糖辅助溶剂热法来构建多孔LiFe_0.4Mn_0.6PO₄/C材料。对比研究两种水热法来制备LiFe_0.4Mn_0.6PO₄/C材料，发现葡萄糖辅助溶剂热法能得到棒状、纳米结构的多孔LiFe_0.4Mn_0.6PO₄/C材料，并表现出优异的电化学性能。在0.1、0.2、0.5、1和2 C时，放电比容量分别达到140.1、130.6、118、106.1和88.9 mAh/g，在1 C倍率下充放电循环100次后保持率达94.7%。这说明在溶剂热法基础上加入一定量的葡萄糖辅助，可以调控制备多孔LiFe_0.4Mn_0.6PO₄/C纳米材料，并能显著改善其倍率性能和循环性能。

关键词：锂离子电池；LiFe_0.4Mn_0.6PO₄/C正极材料；溶剂热法；葡萄糖辅助；电化学性能

中图分类号：O64；TQ174       文献标识码：A         文章编号：0258-3283（2025）07-0043-07

DOI：10.13822/j.cnki.hxsj.2025.0019

Prepation Porous LiFe_0.4Mn_0.6PO₄/C Cathode Material by Glucose Assisted Solvothermal Method  Liu Zhang-bin^1,2, Li Ji-lan^*2  (1.School of Environmental and Chemical Engineering, Dalian University, Dalian 116622, China; 2. School of Chemistry and Materials Engineering, Liupanshui Normal University, Liupanshui 553004, China)

Abstract：Olivine type LiFePO₄ material has become the main positive electrode material for power batteries due to its high theoretical capacity (170 mAh/g), excellent thermal stability, environmental friendliness, and low cost. However, the lower operating voltage of LiFePO₄ (3.4 V vs. Li⁺/Li) results in a lower energy density. Similarly, LiMnPO₄ with an olivine structure has an operating voltage of 4.1 V, resulting in a higher energy density. However, LiMnPO₄ has poor cycling stability. The iron doped LiFe_0.4Mn_0.6PO₄/C material combines the advantages of LiFePO₄ and LiMnPO₄, with high energy density, good cycling stability, and safety, so it has become one of the hot materials in the cathode materials of lithium-ion batteries. However, the rate performance and cycle life of LiFe_0.4Mn_0.6PO_4/C material still need to be further improved before it can be commercially applied. To address these issues, researchers have found that constructing porous structures and carbon coating is one of the most effective methods. For this purpose, glucose assisted solvothermal method was used to prepare porous LiFe_0.4Mn_0.6PO₄/C material in this content. Comparing two hydrothermal methods for preparing LiFe_0.4Mn_0.6PO₄/C materials, it was found that LiFe_0.4Mn_0.6PO₄/C materials prepared by glucose assisted solvothermal method showed rod-shaped and porous nanostructure, which exhibit excellent electrochemical performance, at 0.1、0.2、0.5、1 and 2 C, the discharge specific capacities reached 140.1、130.6、118、106.1 and 88.9 mAh/g, respectively. After 100 charge-discharge cycles at 1 C rate, the retention reached 94.7%. This demonstrates that the structure and morphology of the LiFe_0.4Mn_0.6PO₄/C can be controlled and the rate performance and cycling performance can be significantly improved through glucose-assisted solvothermal synthesis.

Key words：lithium-ion batteries; LiFe_0.4Mn_0.6PO₄/C cathode materials; solvothermal method; glucose assisted; electrochemical performance

BN负载的SnS-Co_1-xS异质结构的制备及其储钠性能研究

徐明远^{1, 2}，王利娟^*1，刘贵龙^*2

（1．辽宁石油化工大学 石油化工学院，辽宁 抚顺  113006；2.洛阳师范学院 化学化工学院，河南 洛阳  471934）

摘要：硫化亚锡（SnS）具有理论容量高、层间距大以及电压平台低等特点，被视为是极具应用前景的钠离子电池（SIBs）负极材料之一。然而，SnS较差的本征导电性及其在循环过程中严重的体积变化，极大地限制了其应用。采用原位生长策略，分别以锡酸钾、六水合氯化钴和硫代乙酰胺为锡源、钴源和硫源，成功制备出氮化硼（BN）负载的SnS-Co_1-xS异质结构负极。利用扫描电子显微镜、透射电子显微镜、X射线衍射和X射线光电子能谱等表征手段，对合成材料进行形貌、结构表征。利用循环伏安测试、恒流充放电测试、阻抗测试和恒电流间歇滴定技术，研究材料的电化学性能和电化学动力学。实验结果表明，BN的引入降低了SnS纳米片的厚度，促进了SnS和Co_1-xS的均匀分散，提供了丰富的SnS-Co_1-xS界面，增强了SnS与Co_1-xS之间的相互作用和电荷转移，从而改善了SnS的本征导电率，并促进了其电化学动力学。所制备的SnS-Co_1-xS/BN电极在2 A/g的电流密度下，比容量为433.9 mAh/g；在0.5 A/g的电流密度下循环200次，比容量高达496.4 mAh/g，表现出较好的倍率性能和循环稳定性。该研究成果提出了一种构筑高性能SnS负极的新策略。

关键词：SnS/Co_1-xS；钠离子电池；BN；负极材料；异质结构

中图分类号：O646             文献标识码：A       文章编号：0258-3283（2025）07-0050-07

DOI：10.13822/j.cnki.hxsj.2025.0043

Preparation and Sodium Storage Performance of BN Supported SnS-Co_1-xS Heterostructure  XU Ming-yuan^1,2, WANG Li-juan^*1, LIU Gui-long^*2(1. School of Petrochemical Engineering, Liaoning Petrochemical Unversity, Fushun 113006, China; 2. College of Chemistry and Chemical Engineering, Luoyang Normal University, Luoyang 471934, China)

Abstract: Tin sulfide (SnS) is regarded as one of the most highly promising anode materials for sodium-ion batteries (SIBs) due to its high theoretical capacity, large interlayer spacing, and suitable voltage platform. However, the poor intrinsic conductivity and the severe volume expansion of SnS during the cycling process have significantly restricted its further application. Boron nitride (BN) supported SnS-Co_1-ₓS heterostructures were obtained via an in situ growth strategy using potassium stannate, cobalt chloride hexahydrate, and thioacetamide as the tin, cobalt, and sulfur sources. The morphology and structure of the synthetic materials were characterized by scanning electron microscope, transmission electron microscope, X-ray diffraction spectrometer, and X-ray photoelectron spectroscopies. The electrochemical performance and electrochemical kinetics of the materials were analyzed through cyclic voltammetry, galvanostatic charge/discharge, impedance, and galvanostatic intermittent titration techniques. The experimental results verified that the introduction of BN reduced the thickness of SnS nanosheets and promoted the uniform dispersion of SnS and Co_1-xS, which provided abundant SnS-Co_1-xS interface and enhanced the interaction and charge transfer between SnS and Co_1-xS, thereby improving the intrinsic conductivity of SnS and accelerating its electrochemical kinetics. As a result, the prepared SnS-Co_1-xS/BN delivered a specific capacity of 433.9 mAh/g at a high current density of 2 A/g and maintained a high specific capacity of 496.4 mAh/g after 200 cycles at 0.5 A/g, showing excellent rate performance and high cycling stability. The research provided a new strategy for constructing high performance SnS anode for SIBs.

Key words: SnS/Co_1-xS; sodium ion battery; BN; anode; heterostructure

对乙酰氨基苯酚的电极过程分析和传感性能研究

 吴子航，陈柳，曹凤娟，王琨琦^*

（长春工程学院 理学院，吉林 长春  130012）

摘要：对乙酰氨基苯酚（PCT）是解热镇痛药物常见成分，用于治疗感冒发热及缓解各种疼痛，过量摄入会引发中毒性肝炎，因此研发快速、精准、成本低廉的检测方法迫在眉睫。鉴于PCT结构特征，构建PCT电化学传感器可以较好的解决上述问题。循环伏安法（CV）是研究耦联均相电化学化学反应的重要技术之一，对揭示药物活性成分的电化学行为及构建高灵敏度电化学传感器具有重要参考价值。以PCT为探针，使用裸玻碳电极为工作电极，通过CV技术系统地考察了PCT在pH 2.4、6.4磷酸氢二钠-柠檬酸缓冲体系和1.80 mol/L硫酸体系中的电化学响应机制，明确了PCT电化学氧化机理，发现了非电化学活性物质的存在，观察到了硫酸介质中耦联均相的电化学反应。利用裸玻碳电极构建了PCT电化学传感器，确定了传感器的线性范围、检出限、灵敏度和选择性等性能参数，对实际药品扑热息痛片进行检测，测得其PCT的含量充足。该检测方法具有简便、快捷和准确的优点。同时，旨在为芳香类有机小分子电极过程动力学提供了关键的实验参考，为芳香类有机小分子药品的快速检测提供方法补充。

关键词：对乙酰氨基苯酚；循环伏安法；裸玻碳电极；耦合均相电化学反应；扑热息痛片；电化学传感器

中图分类号：0657.1         文献标识码：A           文章编号：0258-3283（2025）07-0057-06

DOI：10.13822/j.cnki.hxsj.2025.0099

Electrode Process Analysis and Sensing Performance Research of Acetaminophen WU Zi-hang , CHEN Liu , CAO Feng-juan , WANG Kun-qi^* (Changchun Institute of Technology , School of Science , Changchun , 130012 ,China )

Abstract: Acetaminophen (PCT) is a common ingredient in antipyretic and analgesic drugs for the treatment of cold and fever and the relief of various pains. However, excessive intake can cause toxic hepatitis, making it urgent to development a rapid, accurate, and cost-efficient detection method. Given the structural characteristics of PCT, constructing a PCT electrochemical sensor is an effective solution. Cyclic voltammetry (CV) is one of the important techniques to research coupled homogeneous electrochemical reactions, which is valuable for revealing the electrochemical behavior of pharmaceutical compounds and developing highly sensitive electrochemical sensor. In this study, the electrochemical response mechanism of PCT was systematically investigated using CV with a bare glassy carbon electrode in both pH 2.4 and 6.4 disodium hydrogen phosphate-citric acid buffer system and 1.80 mol/L sulfuric acid system. The oxidization mechanism of PCT was elucidated, non-electrochemically active substances were identified, and the evidence of coupled homogeneous electrochemical reactions of PCT in sulfuric acid medium was observed. The results showed that the electrochemical behavior of PCT is strongly influenced by the acidity of the medium. Based on these findings, a PCT electrochemical sensor was developed using a bare glassy carbon electrode. The performance parameters of the electrochemical sensor, such as the linear range, the detection limit, the sensitivity and the selectivity, were determined. It was successfully applied to detect PCT in commercial paracetamol tablets, confirming adequate content levels. This method has the advantages of simplicity, speed and accuracy. Additionally, this study provides a key experimental insights into the electrode process dynamics of aromatic organic small molecules and complements existing method for the rapid detection in pharmaceutical applications.

Key words: Acetaminophen; cyclic voltammetry (CV); bare glassy carbon electrode; coupled homogeneous electrochemical reaction; paracetamol tablets; Electrochemical sensor

【化学品与环境】

新型环境修复剂磷酸锆材料的研究进展

周靖凯，代雨函，郑钰涛，马佳莹，郝新丽^*，周亚红，秦文婧

（河北地质大学 水资源与环境学院 河北省水资源可持续利用与产业结构优化协同创新中心，河北 石家庄  050031）

摘要：磷酸锆（Zr(HPO₄)₂）是一种重要的层状介孔材料，具有高热稳定性、耐酸碱性以及优异的离子交换性能，广泛应用于多个领域。近年来，磷酸锆这一新型的纳米材料因其独特的物理化学性质正在受到越来越多的关注。围绕磷酸锆纳米材料的晶体形貌、制备方法以及应用领域展开叙述。微纳米结构的磷酸锆材料制备方法多样，目前备受关注的合成方法主要包括溶胶回流法、水热法及配位法等。其中，溶胶回流法操作简单，适合制备层状磷酸锆，可以获得颗粒均匀、纯度高的材料；水热法则能在较低温度下合成磷酸锆。近年来，配位合成法因其高效、节能的特点受到关注，可在短时间内获得结晶性好、粒径分布窄的产物。磷酸锆的应用领域极为广泛。在环境领域，其可用于去除污水中的重金属离子、放射性核废料及有机污染物，表现出良好的吸附性能。此外，磷酸锆还在生物医药、离子交换、催化剂、抗菌材料以及金属表面涂层等方面展现出重要应用价值。随着制备技术的不断优化，磷酸锆的性能和应用范围将进一步拓展，为多领域发展提供支持。

关键词：磷酸锆；层状结构；纳米材料；制备方法；应用领域

中图分类号：O611             文献标识码：A              文章编号：0258-3283（2025）07-0063-08

DOI：10.13822/j.cnki.hxsj.2025.0020

Research Progress of New Environmental Remediation Agent Zirconium Phosphate Materials  ZHOU Jing-kai, DAI Yu-han, ZHENG Yu-tao, MA Jia-ying, HAO Xin-li^*, ZHOU Ya-hong, QIN Wen-jing(Hebei Province Collaborative Innovation Center for Sustainable Utilization of Water Resources and Optimization of Industrial Structure, School of Water Resources & Environment, Hebei GEO University, Shijiazhuang 050031, China)

Abstract：Zirconium phosphate （Zr(HPO₄)₂）is an important layered mesoporous material with high thermal stability, acid and alkali resistance and excellent ion exchange performance, which is widely used in many fields. In recent years, zirconium phosphate, a new type of nanomaterial, has attracted more and more attention due to its unique physical and chemical properties. In this paper, the crystal morphology, preparation methods and application fields of zirconium phosphate nanomaterials are described. There are various preparation methods for micro-nano structured zirconium phosphate materials. At present, the synthesis methods that have attracted much attention mainly include the sol reflux method, hydrothermal method and coordination method. Among them, the sol reflux method is simple and suitable for the preparation of layered zirconium phosphate, which can obtain materials with uniform particles and high purity. The hydrothermal method can synthesize zirconium phosphate at lower temperatures. In recent years, coordination synthesis has attracted much attention due to its high efficiency and energy saving. It can obtain products with good crystallinity and narrow particle size distribution in a short time. Zirconium phosphate has a wide range of application fields. In the environmental field, it can be used to remove heavy metal ions, radioactive nuclear waste and organic pollutants in sewage, showing good adsorption performance. In addition, zirconium phosphate also shows important application value in biomedicine, ion exchange, catalyst, antibacterial material and metal surface coating. With the continuous optimization of preparation technology, the performance and application scope of zirconium phosphate will be further expanded to provide support for multi-field development.

Key words：zirconium phosphate; layer structure；nanomaterials; preparation methods; applications

可循环磁固相萃取-气质联用法测定水中16种PAHs

张文舒^*1，万宇²，王红英¹，吴盼¹

(1.安徽创新检测技术有限公司，安徽 合肥  230094；2. 安徽化工院检测评价科技有限公司，安徽 合肥  230041）

摘要：多环芳烃（PAHs）作为一类典型的持久性有机污染物，广泛存在于水环境中，其具有强致癌性、致突变性及生态毒性，对环境和人类健康构成严重威胁。开发了一种基于可循环磁性复合材料（NiFe₂O₄/SiO₂@PDA）的磁固相萃取（MSPE）结合气相色谱-质谱联用（GC/MS）技术，用于测定水中16种PAHs。通过实验条件的优化，确定最佳萃取条件：磁性材料投加量0.05 g，样品体积15.0 mL，V（正己烷）：V（丙酮）=1:1混合溶液为解吸溶剂，涡旋提取0.5 min、解吸1.0 min。方法学验证结果表明，16种PAHs的线性相关系数（r）均≥0.9995，检出限（LOD）为80~220 ng/L，RSD＜5.0%。实际水样加标实验中，地表水和工业废水的平均回收率为88.0%~114%，RSD为1.5%~5.5%。同时，磁性材料经6次循环使用后，目标物回收率仍保持在90%以上。与文献方法相比，将萃取时间缩短至0.5 min，效率提升30~120倍，同时具有良好的精密度和准确度。方法前处理步骤简单快速、溶剂消耗少、重复性好，适用于水体中痕量PAHs的高效检测，为环境监测提供了一种可靠且环保的分析技术。

关键词：磁固相萃取法；GC/MS；PAHs；可循环；水体

中图分类号：O657        文献标识码：A            文章编号：0258-3283（2025）07-0071-07

DOI：10.13822/j.cnki.hxsj.2025.0002

Determination of 16 PAHs in Water by Recyclable Magnetic Solid-phase Extraction Coupled with GC/MS ZHANG Wen-shu*¹, WAN Yu², WANG Hong-ying¹, WEI Xiao-hu¹, WU Pan¹ (1. Anhui Innovative Testing Technology Co., LTD, Hefei 230094, China; 2. Anhui Chemical Institute Testing and Evaluation Technology Co., LTD, Hefei 230041, China)

Abstract：PAHs, as a class of typical persistent organic pollutants, are widely present in aquatic environments. They exhibit strong carcinogenicity, mutagenicity, and ecotoxicity, posing significant threats to both the environment and human health. This study developed a method based on recyclable magnetic composite materials (NiFe₂O₄/SiO₂@PDA) combined with magnetic solid-phase extraction (MSPE) and gas chromatography-mass spectrometry (GC/MS) for the determination of 16 PAHs in water. Through optimization of experimental conditions, the optimal extraction parameters were determined as follows: magnetic material dosage of 0.05 g, sample volume of 15.0 mL, V(n-hexane):V(acetone) = 1:1 as the desorption solvent, vortex extraction for 0.5 min, and desorption for 1.0 min. Method validation results showed that the linear correlation coefficients (r) for the 16 PAHs were all ≥0.9995, with LOD were 80~20 ng/L and the RSD were ＜5.0%. In spiked experiments with real water samples, the average recovery rates for surface water and industrial wastewater were 88.0%~114 %, with RSDs were 1.5%~5.5 %. Additionally, after six cycles of reuse, the recovery rates of the target compounds remained above 90%. Compared to methods reported in the literature, this approach reduces the extraction time to 0.5 minutes, improving efficiency by 30 to 120 times, while maintaining excellent precision and accuracy. This method features simple and rapid pretreatment steps, low solvent consumption, and good reproducibility, making it suitable for the efficient detection of trace PAHs in water. It provides a reliable and environmentally friendly analytical technique for environmental monitoring.

Key words：MSPE; GC/MS; PAHs; recyclable; water sample

【分析与测试】

库仑滴定法在锌镍镀液中锌含量测定的应用

王岩^a，胡采薇^1b，蔡俊钧^1b，何?^1a，唐俊榕²，程程²，朱志伟^*1b

（1. 北京大学 a. 化学国家级实验教学示范中心；b. 化学与分子工程学院，北京  100871；

2. 上海飞机制造有限公司，上海  201324）

摘要：旨在建立一种适用于复杂锌镍合金镀液体系的锌离子精确定量方法，以突破传统分析技术在该领域的局限性。针对锌镍镀液成分复杂、镍离子干扰显著及配位剂封闭效应等技术瓶颈，创新性地将库仑滴定法与优化标准加入法相结合，构建了基于[Fe(CN)₆]⁴⁻-Zn²⁺沉淀反应的电化学分析体系。该方法通过向待测样品中精确添加过量锌标准溶液，实现双重优化机制：其一，过量锌离子与溶液中共存镍离子形成竞争性沉淀，有效抑制镍离子对锌测定的干扰；其二，饱和配位剂浓度消除其对指示剂的封闭作用，从而省去传统方法的繁琐预处理步骤。通过构建锌标准溶液内标体系，建立库仑滴定终点时间与锌浓度的线性响应关系，采用内标换算方法消除溶液基质效应。研究结果表明，该优化方法不仅显著提高了锌镍镀液中锌含量测定的准确性和效率，还展现出对复杂工业样品体系的强适应性。通过双重控制策略（锌镍物质的量浓度比阈值≥10与标准锌物质的量添加比例1.5~5），成功解决了共沉淀干扰和配位剂封闭的行业难题。为电镀液在线监测技术的开发提供了理论基础，对提升锌镍合金电镀工艺的质量控制具有重要应用价值。

关键词：锌镍镀液；锌含量测定；标准加入法；电分析；库仑滴定法

中图分类号：O657.12        文献标识码：A           文章编号：0258-3283（2025）07-0078-08

DOI：10.13822/j.cnki.hxsj.2025.0036

Application of Coulometric Titration for the Determination of Zinc Content in Zinc-Nickel Plating Solutions WANG Yan^1a, HU Cai-wei^1b, CAI Jun-jun^1b, HE Peng^1a, TANG Jun-rong², CHENG Cheng², ZHU Zhi-wei*^1b(1a. National Demonstration Center for Experimental Chemistry Education, 1b. College of Chemistry and Molecular Engineering, Beijing 100871, China; 2. Shanghai Aircraft Manufacturing Co. Ltd., Shanghai 201324, China)

Abstract: This study presents a novel analytical strategy for precise zinc ion quantitation in complex zinc-nickel plating solutions, overcoming the limitations of conventional techniques in this field. Targeting technical bottlenecks such as solution complexity, nickel ion interference, and ligand blocking effects, we integrated coulometric titration with an optimized standard addition method, establishing an electrochemical analysis system based on the [Fe(CN)₆]^4--Zn²⁺ precipitation reaction. The dual optimization mechanism involves: (i) competitive precipitation suppression of nickel interference through excess zinc addition, and (ii) saturation of ligand binding sites to eliminate indicator blocking, thereby eliminating tedious pretreatment procedures. An internal standard system using zinc standards enabled linear calibration between coulometric titration endpoint time and concentration, with matrix effects corrected through internal standard conversion algorithms. The optimized method not only significantly enhances accuracy and efficiency for zinc determination in industrial plating solutions, but also shows strong adaptability to complex industrial sample systems. By implementing dual control strategies (Zn/Ni molarity ratio ≥ 10 and standard addition ratio 1.5~5), we resolved co-precipitation interference and ligand blocking challenges. This work provides theoretical foundations for developing online monitoring technologies, offering practical value for quality control in zinc-nickel alloy electroplating processes.

Key words：zinc-nickel plating solutions; zinc content determination; standard addition method; electroanalysis; coulometric titration

基于MOF-808(Zr)的表面分子印迹荧光传感器的制备

及其对槲皮素的检测

王宇，李媛媛^*，黄浩展，邢建平，王天聪，王茜，张茜莹，牛浩宇，何娟

(河南工业大学 化学化工学院，河南 郑州  450001 )

摘要：槲皮素是一种存在于中草药、水果和蔬菜中的天然黄酮类化合物，具有抗氧化、抗炎等生物学特性。然而，槲皮素的过量摄入会对人体造成危害，因此探索一种简便、快速、有效的检测方法测定食品中槲皮素的含量至关重要。以金属有机框架MOF-808(Zr)为载体，有机荧光分子四苯基吡嗪衍生物（TPP）为荧光基团，采用沉淀聚合法制备了一种可用于槲皮素检测的表面分子印迹荧光传感器（MOF-808-TPP@SMIPs）。采用傅里叶变换红外光谱、扫描电子显微镜及X射线衍射等技术对传感器进行表征，表明已经成功合成。传感器在较短时间内可以实现槲皮素的吸附平衡。在检测槲皮素时，其荧光强度比值（F₀/F）与槲皮素在0.6 ~ 10 μmol/L的浓度范围内呈现良好的线性关系（相关系数R²=0.9983），检出限为0.18 μmol/L。此外，MOF-808-TPP@SMIPs具有高选择性、良好的重复使用性和稳定的荧光性能等特点。采用本传感器对实际样品进行检测时，槲皮素的回收率为86.78% ~ 107.65%，相对标准偏差为1.08% ~ 5.50%，表明其可以用于实际样品中槲皮素的检测。该研究为槲皮素的高效快速检测提供了一种可行的方法。

关键词：表面分子印迹聚合物；荧光传感器；四苯基吡嗪衍生物；槲皮素；MOF-808(Zr)

中图分类号：O65              文献标识码：A              文章编号：0258-3283（2025）07-0086-07

DOI：10.13822/j.cnki.hxsj.2025.0065

Preparation of MOF-808(Zr)-Based Surface Molecularly Imprinted Fluorescence Sensor for Quercetin Detection  WANG Yu, LI Yuan-yuan^*, HUANG Hao-zhan, XING Jian-ping, WANG Tian-cong, WANG Xi, ZHANG Xi-ying, NIU Hao-yu, HE Juan (School of Chemistry and Chemical Engineering, Henan University of Technology, Zhengzhou 450001, China) 

Abstract: Quercetin is a natural flavonoid compound found in Chinese herbal medicines, fruits and vegetables, which has biological properties such as antioxidation and anti-inflammation. However, excessive intake of quercetin can cause harm to the human body. Therefore, it is of vital importance to explore a simple, rapid and effective detection method for determining the content of quercetin in food. By using metal-organic framework MOF-808(Zr) as the carrier, tetraphenylpyrazine derivative (TPP) as the fluorophore, a surface molecularly imprinted fluorescence sensor (MOF-808-TPP@SMIPs) for quercetin detection was prepared by precipitation polymerization. The sensor was characterized by Fourier-transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM), and X-ray diffraction (XRD), which confirmed the successful preparation of the sensor. The sensor can achieve the adsorption equilibrium of quercetin in a relatively short period of time. The fluorescence intensity ratios (F₀/F) showed a linear relationship with the concentrations of quercetin in the range of 0.6~10 μmol/L (R²=0.9983) with a detection limit of 0.18 μmol/L. The sensor also exhibited the advantages of high selectivity, excellent reusability, and good fluorescence stability. The recoveries of quercetin in real samples detected by this sensor ranged from 86.78% to 107.65% with the relative standard deviations of 1.08%~5.50%, which indicated that it can be apply in the detection of quercetin in real samples. This study provided a feasible method for efficient and rapid detection of quercetin.

Key words：surface molecularly imprinted polymers; fluorescence sensor; tetraphenylpyrazine derivative; quercetin; MOF-808(Zr)

基于GC-MS法同时测定卷烟主流烟气中30种有机酸释放量

惠非琼，银芳，张丽，魏建科，胡芸，王伟国，张小涛，谢顺萍，赵杨，姬厚伟^*

（贵州中烟工业有限责任公司技术中心,贵州 贵阳  550009）

摘要：为了高效、准确的测定卷烟主流烟气30种有机酸释放量，基于涡旋振荡萃取结合气相色谱-质谱联用（GC/MS），通过优化前处理萃取和色谱条件，采用极性DB-FFAP毛细管柱，建立同时测定卷烟主流烟气中甲酸、乙酸、巴豆酸、油酸、糠酸、硬脂酸和二十酸等30种挥发半挥发性有机酸释放量分析方法。卷烟在标准抽吸模式下，采用剑桥滤片捕集卷烟主流烟气粒相物，依次添加反式-2-己烯酸、十六酸-d₃₁内标和萃取溶剂甲醇后，涡旋振荡萃取，采用选择离子监测模式下 GC/MS内标法定量分析。本方法30种有机酸的检出限（LOD）和定量限（LOQ）分别为0.002~0.96 μg/支和0.01~3.2 μg/支，且在线性范围内线性关系较好，线性相关系数R²均大于0.999；加标回收率为 91.1%~106.6%，RSD为 0.4%~7.9%。本方法前处理简单、高效、灵敏，适用于不同类型卷烟主流烟气粒相物中甲酸、乙酸、巴豆酸、油酸、糠酸、硬脂酸和二十酸等30种挥发半挥发性有机酸释放量的测定，可以精准调控烟用材料参数设计及不同配方的烟用香精香料使用量对卷烟烟气有机酸释放量的影响，为卷烟产品设计、自主调香、风格特征评价提供关键技术支撑。

关键词：气相色谱?质谱；卷烟主流烟气；涡旋振荡萃取；甲醇；有机酸；释放量

中图分类号：O657        文献标识码：A      文章编号：0258-3283（2025）07-0093-09

DOI：10.13822/j.cnki.hxsj.2025.0014

Release of 30 Kinds of Organic Acids in Mainstream Cigarette Smoke Simultaneously Determined by GC/MS HUI Fei-qiong, YIN Fang, ZHANG Li, WEI Jian-ke, HU Yun, WANG Wei-guo, ZHANG Xiao-tao, XIE Shun-ping, ZHAO Yang, JI Hou-wei^*（Technology Center, China Tobacco Guizhou Industrial Co., Ltd, Guiyang 550009, China）

Abstract: In order to determine the release of 30 kinds of organic acids from mainstream cigarette smoke efficiently and accurately, a novel method for simultaneous determination of 30 volatile organic acids, including formic acid, acetic acid, crotonic acid, oleic acid, furoic acid, stearic acid and eicosic acid, was developed by using polar DB-FFAP capillary column based on vortex extraction combined with gas chromatography-mass spectrometry (GC/MS). In the standard smoking mode, the TPMs of cigarettes were captured by Cambridge filter, and the internal standard of trans-2-hexenic acid and hexanoic acid-d₃₁ were added, then extracted by methanol vortex oscillation, and quantitatively analyzed by GC/MS in the selective ion monitoring mode. The LOD and LOQ of 30 organic acids were 0.012~0.96 μg/ branch and 0.01~3.2 μg/ branch, respectively, and the good linear relationships were presented in the linear range (R²≥0.999). The recoveries and the relative standard deviations(RSD%) of 30 organic acids were 91.1%~106.6% and 0.4%~7.9%, respectively. The method is simple, efficient and sensitive, and is suitable for the determination of the release amount of 30 volatile and semi-volatile organic acids such as formic acid, acetic acid, crotonic acid, oleic acid, furoic acid, stearic acid and eicosic acid in the particle phase of the mainstream smoke of different types of cigarettes. It can accurately control the design of tobacco material parameters and the influence of the amount of tobacco flavors and spices used in different formulations on the organic acid release amount of cigarette smoke. It provides key technical support for cigarette product design, independent aroma modulation and style characteristic evaluation.

Key words: gas chromatography-mass spectrometry;mainstream cigarette smoke; vortex extraction; methanol; organic acids; release

UHPLC-MS/MS-QAMS法测定金丹附延颗粒中4种生物碱含量

朱良辉¹，吴倩颖^1,2，陈伟康^*，刘德鸿¹，陈希¹，缪贵忠³

（1. 江西省药品检验检测研究院 国家药品监督管理局中成药质量评价重点实验室 江西省药品医疗器械质量工程研究中心，江西 南昌  330029；2.江西中医药大学，江西 南昌  330004；3.江西华太药业有限公司，江西 宜丰  336300）

摘 要：采用液质联用结合一测多评技术建立同时测定金丹附延颗粒中原阿片碱、延胡索乙素、海罂粟碱、延胡索甲素含量的一测多评方法。采用超高效液相色谱，Waters BEH C18 （2.1 mm×100 mm，1.7 μm）色谱柱，以乙腈-含5 mmoL/mL甲酸铵的0.1%甲酸溶液为流动相，流速 0.3 mL/min，梯度洗脱。质谱采用电喷雾离子源，正离子多反应监测模式，监测离子对为：原阿片碱354.3/188、延胡索乙素356.2/192、海罂粟碱356.3/325.1、延胡索甲素370.2/191.8；以延胡索乙素为内参物，两个品牌液质联用仪，3个品牌的色谱柱作为耐用性考察比较因素，计算不同仪器和不同色谱柱测得相对校正因子的相对标准偏差；采用一测多评（QAMS）法计算4个生物碱成分含量，结果与外标法进行比较。4个生物碱在浓度 10~1000 ng/mL范围内线性关系良好，r＞0.9961，重现性、回收率等方法考察均符合要求，方法耐用性好，QAMS法和外标法结果无显著性差异。该方法节可节省对照品开支，有效降低检验成本，测试时间短、灵敏度高、专属性良好，可用于金丹附延颗粒中原阿片碱、延胡索乙素、海罂粟碱、延胡索甲素含量测定。

关键词：金丹附延颗粒；原阿片碱；延胡索乙素；海罂粟碱；延胡索甲素；一测多评；液质联用

中图分类号：O657       文献标识码：A          文章编号：0258-3283（2025）07-0102-06

DOI：10.13822/j.cnki.hxsj.2025.0018

Determination of Four Alkaloids in Jindanfuyan Granules by UHPLC-MS/MS-QAMS  ZHU Liang-hui¹, WU Qian-ying^1,2, CHEN Wei-kang*¹，LIU De-hong¹, CHEN Xi¹，MIAO Gui-zhong³（1.Jiangxi Institute for Drug Control, NMPA Key Laboratory of Quality Evaluation of Traditional Chinese Patent Medicine, Jiangxi Province Engineering Research Center of Drug and Medical Device Quality, Nanchang Jiangxi 330029, China; 2.Jiangxi University of Traditional Chinese Medicine, Nanchang Jiangxi 330029, China ；3.Jiangxi Huatai Pharmaceutical Co., LTD，Yifeng Jiangxi 336300, China）

Abstract：A UHPLC-MS/MS-QAMS method was established for simultaneous determination of  protopine，tetrahydropalmatine，glaucine and corydaline in Jindanfuyan granules. Ultra-high-performance liquid chromatography was adopted with a Waters BEH C₁₈ （2.1×100 mm，1.7 μm） column，and the mobile phase consisted of acetonitrile and 0.1% formic acid containing 5 mmol/mL ammonium formate.The flow rate was set at 0.3 mL/min with gradient elution. The mass spectrometry equiped an electrospray ionization source, positive multi-reaction monitoring mode, and the monitored ion pairs were:  protopine 354.3/188，tetrahydropalmatine 356.2/192，glaucine 356.3/325.1 and corydaline 370.2/191.8. Using tetrahydropalmatine as the internal reference substance, the relative standard deviations of the relative correction factors measured by two brands of liquid chromatography - mass spectrometry (LC - MS) instruments and three brands of chromatographic columns were calculated as the factor for the durability investigation. The contents of four alkaloid components were calculated by the quantitative analysis of QAMS method, and the results were compared with those obtained by the external standard method. The four alkaloids have a good linear relationship in the concentration range of 10~1000 ng/mL (r > 0.9961). The reproducibility and recovery of the four alkaloids are within the acceptable ranges. The contents of the four alkaloids are no significant differences between the QAMS and the external standard method. The method has good durability with methodological evaluations with high sensitivity，good specificity and the advantages of short test time. It can be used for the determination of protopine，tetrahydropalmatine，glaucine and corydaline in Jindanfuyan granules.

Key words：Jindanfuyan Granules; protopine; tetrahydropalmatine; glaucine; corydaline; QAMS; UHPLC-MS/MS