{"title":"基于浮式深共熔溶剂固化的涡辅助分散液-液微萃取法(VA-DLLME-SFDES) HPLC测定中药中酒石黄的建立与验证:基于分析生态标度的绿色剖面评价","authors":"Qingqing Cao, Huinan Cui, Mengli Wu, Rongling Wang, Yaxuan Chen, Qingxin Zhao, Junmei Li","doi":"10.1016/j.microc.2025.115096","DOIUrl":null,"url":null,"abstract":"<div><div>In this work, a novel and environmentally friendly vortex-assisted dispersive liquid-liquid microextraction based on solidification of floating deep eutectic solvent (VA-DLLME-SFDES) coupled with high performance liquid chromatography-ultraviolet detector (HPLC-UV) was developed to determine tartrazine illegally added in traditional Chinese medicine for the first time. A deep eutectic solvent (DES) composed of tetrabutylammonium chloride as the hydrogen bond acceptor (HBA) and octanoic acid as the hydrogen bond donor (HBD) at a molar ratio of 1:2 was selected as the extractant. Vortex mixing was employed to accelerate the dispersion of DES droplets into the sample phase. Following centrifugation, solvent solidification was employed to facilitate the collection of the DES phase, thereby increasing recovery and reproducibility. Subsequently, the upper DES phase was melted at room temperature for further HPLC analysis. Factors affecting VA-DLLME-SFDES, such as the type of DES, volume of DES, vortex time, centrifugal speed, pH value, salt effect, and solidification time, were systematically investigated. Under the optimum extraction conditions, the developed method was successfully applied for the determination of tartrazine illegally added in three traditional Chinese medicines. The calibration curve of tartrazine was linear in the range of 2.044–408.8 ng mL<sup>−1</sup> (<em>r</em> ≥ 0.9996). The limit of quantification (LOQ) and limit of detection (LOD) were 2.044 ng mL<sup>−1</sup> and 0.5110 ng mL<sup>−1</sup>, respectively. The recoveries ranged from 97.5 % to 102.3 % with relative standard deviations (RSDs) lower than 2.0 %. Finally, the ecological impact was evaluated using Analytical Eco-Scale (AES). The results demonstrate that this method offers significant advantages, including simplicity, rapidity, low cost, high sensitivity, and environmental friendliness. It is suitable for analyzing tartrazine illegally added in traditional Chinese medicine and shows promising potential for broader applications in detecting other trace analytes in complex matrices.</div></div>","PeriodicalId":391,"journal":{"name":"Microchemical Journal","volume":"218 ","pages":"Article 115096"},"PeriodicalIF":4.9000,"publicationDate":"2025-09-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"0","resultStr":"{\"title\":\"Development and validation of vortex-assisted dispersive liquid-liquid microextraction based on solidification of floating deep eutectic solvent (VA-DLLME-SFDES) for determination of tartrazine in traditional Chinese medicine by HPLC: Green profile assessment using analytical eco-scale\",\"authors\":\"Qingqing Cao, Huinan Cui, Mengli Wu, Rongling Wang, Yaxuan Chen, Qingxin Zhao, Junmei Li\",\"doi\":\"10.1016/j.microc.2025.115096\",\"DOIUrl\":null,\"url\":null,\"abstract\":\"<div><div>In this work, a novel and environmentally friendly vortex-assisted dispersive liquid-liquid microextraction based on solidification of floating deep eutectic solvent (VA-DLLME-SFDES) coupled with high performance liquid chromatography-ultraviolet detector (HPLC-UV) was developed to determine tartrazine illegally added in traditional Chinese medicine for the first time. A deep eutectic solvent (DES) composed of tetrabutylammonium chloride as the hydrogen bond acceptor (HBA) and octanoic acid as the hydrogen bond donor (HBD) at a molar ratio of 1:2 was selected as the extractant. Vortex mixing was employed to accelerate the dispersion of DES droplets into the sample phase. Following centrifugation, solvent solidification was employed to facilitate the collection of the DES phase, thereby increasing recovery and reproducibility. Subsequently, the upper DES phase was melted at room temperature for further HPLC analysis. Factors affecting VA-DLLME-SFDES, such as the type of DES, volume of DES, vortex time, centrifugal speed, pH value, salt effect, and solidification time, were systematically investigated. Under the optimum extraction conditions, the developed method was successfully applied for the determination of tartrazine illegally added in three traditional Chinese medicines. The calibration curve of tartrazine was linear in the range of 2.044–408.8 ng mL<sup>−1</sup> (<em>r</em> ≥ 0.9996). The limit of quantification (LOQ) and limit of detection (LOD) were 2.044 ng mL<sup>−1</sup> and 0.5110 ng mL<sup>−1</sup>, respectively. The recoveries ranged from 97.5 % to 102.3 % with relative standard deviations (RSDs) lower than 2.0 %. Finally, the ecological impact was evaluated using Analytical Eco-Scale (AES). The results demonstrate that this method offers significant advantages, including simplicity, rapidity, low cost, high sensitivity, and environmental friendliness. It is suitable for analyzing tartrazine illegally added in traditional Chinese medicine and shows promising potential for broader applications in detecting other trace analytes in complex matrices.</div></div>\",\"PeriodicalId\":391,\"journal\":{\"name\":\"Microchemical Journal\",\"volume\":\"218 \",\"pages\":\"Article 115096\"},\"PeriodicalIF\":4.9000,\"publicationDate\":\"2025-09-03\",\"publicationTypes\":\"Journal Article\",\"fieldsOfStudy\":null,\"isOpenAccess\":false,\"openAccessPdf\":\"\",\"citationCount\":\"0\",\"resultStr\":null,\"platform\":\"Semanticscholar\",\"paperid\":null,\"PeriodicalName\":\"Microchemical Journal\",\"FirstCategoryId\":\"92\",\"ListUrlMain\":\"https://www.sciencedirect.com/science/article/pii/S0026265X25024440\",\"RegionNum\":2,\"RegionCategory\":\"化学\",\"ArticlePicture\":[],\"TitleCN\":null,\"AbstractTextCN\":null,\"PMCID\":null,\"EPubDate\":\"\",\"PubModel\":\"\",\"JCR\":\"Q1\",\"JCRName\":\"CHEMISTRY, ANALYTICAL\",\"Score\":null,\"Total\":0}","platform":"Semanticscholar","paperid":null,"PeriodicalName":"Microchemical Journal","FirstCategoryId":"92","ListUrlMain":"https://www.sciencedirect.com/science/article/pii/S0026265X25024440","RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"Q1","JCRName":"CHEMISTRY, ANALYTICAL","Score":null,"Total":0}
引用次数: 0
摘要
本文首次建立了一种新型的环境友好型涡流辅助分散液液微萃取方法,该方法基于浮式深共晶溶剂(VA-DLLME-SFDES)固化,并结合高效液相色谱-紫外检测器(HPLC-UV)测定中药中非法添加的酒石黄。选择四丁基氯化铵为氢键受体(HBA),辛酸为氢键给体(HBD),摩尔比为1:2的深共晶溶剂(DES)作为萃取剂。采用涡旋混合加速了DES液滴在样品相中的分散。离心后,溶剂固化有利于DES相的收集,从而提高回收率和重现性。随后,在室温下将上DES相熔化以进行进一步的HPLC分析。系统研究了影响VA-DLLME-SFDES的因素,如DES类型、DES体积、漩涡时间、离心速度、pH值、盐效应、凝固时间等。在最佳提取条件下,本法成功地测定了三种中药中非法添加的酒黄石。酒黄石在2.044 ~ 408.8 ng mL−1范围内呈线性关系(r≥0.9996)。定量限(LOQ)和检出限(LOD)分别为2.044 ng mL - 1和0.5110 ng mL - 1。加样回收率为97.5% ~ 102.3%,相对标准偏差(rsd)小于2.0%。最后,采用分析生态尺度法(AES)对生态影响进行评价。结果表明,该方法具有简单、快速、成本低、灵敏度高、环境友好等优点。该方法适用于分析中药中非法添加的酒黄石,在复杂基质中其他痕量分析物的检测方面具有广阔的应用前景。
Development and validation of vortex-assisted dispersive liquid-liquid microextraction based on solidification of floating deep eutectic solvent (VA-DLLME-SFDES) for determination of tartrazine in traditional Chinese medicine by HPLC: Green profile assessment using analytical eco-scale
In this work, a novel and environmentally friendly vortex-assisted dispersive liquid-liquid microextraction based on solidification of floating deep eutectic solvent (VA-DLLME-SFDES) coupled with high performance liquid chromatography-ultraviolet detector (HPLC-UV) was developed to determine tartrazine illegally added in traditional Chinese medicine for the first time. A deep eutectic solvent (DES) composed of tetrabutylammonium chloride as the hydrogen bond acceptor (HBA) and octanoic acid as the hydrogen bond donor (HBD) at a molar ratio of 1:2 was selected as the extractant. Vortex mixing was employed to accelerate the dispersion of DES droplets into the sample phase. Following centrifugation, solvent solidification was employed to facilitate the collection of the DES phase, thereby increasing recovery and reproducibility. Subsequently, the upper DES phase was melted at room temperature for further HPLC analysis. Factors affecting VA-DLLME-SFDES, such as the type of DES, volume of DES, vortex time, centrifugal speed, pH value, salt effect, and solidification time, were systematically investigated. Under the optimum extraction conditions, the developed method was successfully applied for the determination of tartrazine illegally added in three traditional Chinese medicines. The calibration curve of tartrazine was linear in the range of 2.044–408.8 ng mL−1 (r ≥ 0.9996). The limit of quantification (LOQ) and limit of detection (LOD) were 2.044 ng mL−1 and 0.5110 ng mL−1, respectively. The recoveries ranged from 97.5 % to 102.3 % with relative standard deviations (RSDs) lower than 2.0 %. Finally, the ecological impact was evaluated using Analytical Eco-Scale (AES). The results demonstrate that this method offers significant advantages, including simplicity, rapidity, low cost, high sensitivity, and environmental friendliness. It is suitable for analyzing tartrazine illegally added in traditional Chinese medicine and shows promising potential for broader applications in detecting other trace analytes in complex matrices.
期刊介绍:
The Microchemical Journal is a peer reviewed journal devoted to all aspects and phases of analytical chemistry and chemical analysis. The Microchemical Journal publishes articles which are at the forefront of modern analytical chemistry and cover innovations in the techniques to the finest possible limits. This includes fundamental aspects, instrumentation, new developments, innovative and novel methods and applications including environmental and clinical field.
Traditional classical analytical methods such as spectrophotometry and titrimetry as well as established instrumentation methods such as flame and graphite furnace atomic absorption spectrometry, gas chromatography, and modified glassy or carbon electrode electrochemical methods will be considered, provided they show significant improvements and novelty compared to the established methods.