[非水毛细管电泳法同时测定消毒剂、个人护理用品和润肤油中三氯生、三氯卡班和对氯间二甲酚]。

IF 1.2 4区 化学 Q4 CHEMISTRY, ANALYTICAL 色谱 Pub Date : 2023-02-01 DOI:10.3724/SP.J.1123.2022.06016
Ruoke Jiang, Xiaojing Ding
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However, the results analyzed according to the National Standard method often exceed the declared contents, thereby indicating the necessity to establish a new method based on a completely different principle (e. g., capillary electrophoresis), especially since it was not possible to analyze TCS, TCC, and PCMX in a single injection using the National Standard method. Moreover, using this method, large amounts of methanol were consumed, which could be potentially harmful to both operators and the environment. In terms of their water solubilities, this decreases in the order of PCMX>TCS>TCC, wherein TCC is insoluble in water. As such, the use of nonaqueous capillary electrophoresis (NACE) based on running buffer solutions prepared in pure organic solvents (e. g., methanol or acetonitrile) is necessary. In this paper, a new NACE approach combined with an ultraviolet detection method was developed for the simultaneous analysis of TCS, TCC, and PCMX in disinfectants, personal care products, and ointments. For this purpose, an uncoated fused silica capillary (20 cm×50 μm, total length=30.2 cm) was used as the separation column with a separation buffer composed of 14 mmol/L sodium borate, 2 g/L polyethylene glycol (PEG) 20000, and 0.5 mmol/L dodecyltrimethylammonium bromide (DTAB) in methanol. Following optimization of the separation parameters, the complete and simultaneous separation of TCS, TCC, and PCMX was achieved when the sample solution was prepared using 5 g/L PEG 20000 in methanol-acetonitrile (50∶50, v/v). It was possible to directly inject the sample into the analysis system after a simple dilution with the sample medium, and no interference was observed in any of the sample electropherograms when a separation voltage and detection wavelength of -12 kV and 214 nm were employed, respectively. Furthermore, TCS, TCC, and PCMX showed good linear relationships with their corrected peak areas within a mass concentration range of 1-100 mg/L, and the correlation coefficients (<i>r</i>) were all greater than 0.99. Moreover, the limits of detection (LODs, <i>S/N</i>=3) and limits of quantification (LOQs, <i>S/N</i>=10) were determined to be 0.2 and 1 mg/L, respectively. The spiked recoveries ranged from 94.5% to 104.4% with relative standard deviations of ≤4.8% in all cases. Subsequently, the established method was used to analyze 31 commercial samples, including hand sanitizer, disinfectant, baby powder, and antibacterial cream. 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引用次数: 1

摘要

三氯生(TCS)、三氯卡班(TCC)和对氯-间二甲酚(PCMX)因其广谱、高效的杀菌作用而成为应用最广泛的抗生素。在消毒方面,国家标准GB 38598-2020规定了消毒剂中有效成分的含量,其范围必须在规定的中心值的90%-110%之间。为保证合适的产品质量,GB/T 27947-2020和GB/T 34856-2017建议采用高效液相色谱法进行分析。然而,根据国家标准方法分析的结果往往超过声明的内容,这表明有必要建立一种基于完全不同原理的新方法。例如,毛细管电泳),特别是因为不可能使用国家标准方法分析一次注射中的TCS, TCC和PCMX。此外,使用这种方法会消耗大量的甲醇,这可能对操作人员和环境都有潜在的危害。其水溶性大小为PCMX>TCS>TCC,其中TCC不溶于水。因此,使用非水毛细管电泳(NACE)的基础上运行缓冲溶液制备的纯有机溶剂(e。(如甲醇或乙腈)是必要的。本文建立了一种新的NACE结合紫外检测法同时分析消毒剂、个人护理用品和软膏中TCS、TCC和PCMX的方法。采用无包被熔融石英毛细管(20 cm×50 μm,总长30.2 cm)作为分离柱,分离缓冲液由14 mmol/L硼酸钠、2 g/L聚乙二醇(PEG) 20000、0.5 mmol/L十二烷基三甲基溴化铵(DTAB)甲醇组成。通过对分离参数的优化,在5 g/L PEG 20000的甲醇-乙腈(50∶50,v/v)溶液中制备样品溶液时,实现了TCS、TCC和PCMX的完全同时分离。当分离电压为-12 kV,检测波长为214 nm时,样品经简单的样品介质稀释后可直接注入分析系统,样品的电泳图均无干扰。在1 ~ 100 mg/L的质量浓度范围内,TCS、TCC和PCMX与其校正峰面积呈良好的线性关系,相关系数(r)均大于0.99。检测限(lod, S/N=3)为0.2 mg/L,定量限(loq, S/N=10)为1 mg/L。加标回收率为94.5% ~ 104.4%,相对标准偏差≤4.8%。随后,使用建立的方法分析了31个商业样品,包括洗手液、消毒剂、婴儿爽身粉和抗菌乳膏。采用高效液相色谱法(HPLC)、NACE法和MEKC法对TCS、TCC和PCMX进行了定量分析。虽然三种方法之间没有统计学上的显著差异,但31个样品中有16个样品的测定结果与声称的含量不符。因此,有必要进一步控制消毒产品的成分。我们的研究结果表明,新建立的NACE方法可以成为常规实验室分析的重要替代方法,特别是考虑到它可以最大限度地减少废物产生,只需要简单的样品预处理过程,并且对目标化合物具有良好的选择性。因此,希望在不久的将来将NACE方法纳入国家标准方法。
本文章由计算机程序翻译,如有差异,请以英文原文为准。

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[Simultaneous determination of triclosan,triclocarban and p-chloro-m-xylenol in disinfectant,personal care products and oiltment by nonaqueous capillary electrophoresis].

Triclosan (TCS), triclocarban (TCC), and p-chloro-m-xylenol (PCMX) are some of the most widely used antibiotics because of their broad-spectrum and highly-efficient bactericidal effects. In the context of disinfection, the National Standard GB 38598-2020 stipulates that the contents of the effective ingredients present in a disinfectant must be specified, wherein their range must fall within 90%-110% of the specified central value. To ensure a suitable product quality, analysis by high performance liquid chromatography (HPLC) is recommended by both the GB/T 27947-2020 and GB/T 34856-2017. However, the results analyzed according to the National Standard method often exceed the declared contents, thereby indicating the necessity to establish a new method based on a completely different principle (e. g., capillary electrophoresis), especially since it was not possible to analyze TCS, TCC, and PCMX in a single injection using the National Standard method. Moreover, using this method, large amounts of methanol were consumed, which could be potentially harmful to both operators and the environment. In terms of their water solubilities, this decreases in the order of PCMX>TCS>TCC, wherein TCC is insoluble in water. As such, the use of nonaqueous capillary electrophoresis (NACE) based on running buffer solutions prepared in pure organic solvents (e. g., methanol or acetonitrile) is necessary. In this paper, a new NACE approach combined with an ultraviolet detection method was developed for the simultaneous analysis of TCS, TCC, and PCMX in disinfectants, personal care products, and ointments. For this purpose, an uncoated fused silica capillary (20 cm×50 μm, total length=30.2 cm) was used as the separation column with a separation buffer composed of 14 mmol/L sodium borate, 2 g/L polyethylene glycol (PEG) 20000, and 0.5 mmol/L dodecyltrimethylammonium bromide (DTAB) in methanol. Following optimization of the separation parameters, the complete and simultaneous separation of TCS, TCC, and PCMX was achieved when the sample solution was prepared using 5 g/L PEG 20000 in methanol-acetonitrile (50∶50, v/v). It was possible to directly inject the sample into the analysis system after a simple dilution with the sample medium, and no interference was observed in any of the sample electropherograms when a separation voltage and detection wavelength of -12 kV and 214 nm were employed, respectively. Furthermore, TCS, TCC, and PCMX showed good linear relationships with their corrected peak areas within a mass concentration range of 1-100 mg/L, and the correlation coefficients (r) were all greater than 0.99. Moreover, the limits of detection (LODs, S/N=3) and limits of quantification (LOQs, S/N=10) were determined to be 0.2 and 1 mg/L, respectively. The spiked recoveries ranged from 94.5% to 104.4% with relative standard deviations of ≤4.8% in all cases. Subsequently, the established method was used to analyze 31 commercial samples, including hand sanitizer, disinfectant, baby powder, and antibacterial cream. A comparative analysis of HPLC, the developed NACE method, and our previously reported micellar electrokinetic chromatographic (MEKC) method was also carried out for the quantitative determination of TCS, TCC, and PCMX. Although no statistically significant differences were observed among the three methods, the results determined for 16 out of the 31 samples did not match the claimed contents. These results therefore indicate the necessity to further control the compositions of disinfectant products. Our results indicate that the newly established NACE method can be an important alternative to HPLC for routine laboratory analyses, especially considering that it minimizes waste generation, requires only a simple sample pretreatment process, and exhibits a good selectivity to the target compounds. It is therefore hoped that the NACE method will be incorporated into the National Standard method in the near future.

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来源期刊
色谱
色谱 CHEMISTRY, ANALYTICAL-
CiteScore
1.30
自引率
42.90%
发文量
7198
期刊介绍: "Chinese Journal of Chromatography" mainly reports the basic research results of chromatography, important application results of chromatography and its interdisciplinary subjects and their progress, including the application of new methods, new technologies, and new instruments in various fields, the research and development of chromatography instruments and components, instrument analysis teaching research, etc. It is suitable for researchers engaged in chromatography basic and application technology research in scientific research institutes, master and doctoral students in chromatography and related disciplines, grassroots researchers in the field of analysis and testing, and relevant personnel in chromatography instrument development and operation units. The journal has columns such as special planning, focus, perspective, research express, research paper, monograph and review, micro review, technology and application, and teaching research.
期刊最新文献
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