方法文章

A Two-Step Pyrolysis-Gas Chromatography Method with Mass Spectrometric Detection for Identification of Tattoo Ink Ingredients and Counterfeit Products

DOI：

10.3791/59689

⸱

2019年5月22日

 ,  , 
1Department of Chemical and Product Safety, German Federal Institute for Risk Assessment (BfR)

本文内容

摘要

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This method for two-step pyrolysis online coupled to gas chromatography with mass spectrometric detection and data evaluation protocol can be used for multi-component analysis of tattoo inks and discrimination of counterfeit products.

摘要

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Tattoo inks are complex mixtures of ingredients. Each of them possesses different chemical properties which have to be addressed upon chemical analysis. In this method for two-step pyrolysis online coupled to gas chromatography mass spectrometry (py-GC-MS) volatile compounds are analyzed during a first desorption run. In the second run, the same dried sample is pyrolyzed for analysis of non-volatile compounds such as pigments and polymers. These can be identified by their specific decomposition patterns. Additionally, this method can be used to differentiate original from counterfeit inks. Easy screening methods for data evaluation using the average mass spectra and self-made pyrolysis libraries are applied to speed up substance identification. Using specialized evaluation software for pyrolysis GS-MS data, a fast and reliable comparison of the full chromatogram can be achieved. Since GC-MS is used as separation technique, the method is limited to volatile substances upon desorption and after pyrolysis of the sample. The method can be applied for quick substance screening in market control surveys since it requires no sample preparation steps.

引言

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Tattoo inks are complex mixtures consisting of pigments, solvents, binders, surfactants, thickening agents, and, sometimes, preservatives1. The increased popularity of tattooing in the last decades has led to the establishment of legislation addressing tattoo ink safety across Europe. In most instances, color-giving pigments and their impurities are restricted and therefore should be monitored by state laboratory market surveys to control their compliance with law.

Using the approach of online pyrolysis-gas chromatography mass spectrometry (py-GC-MS) described here, multiple ingredients can be identified simultaneous....

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方案

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1. Tattoo ink preparation and sample mounting

  1. Use a 25 mm hollow glass pyrolysis tube as a sample holder and quartz wool for sample preparation.
    1. Grab the pyrolysis tube with the specialized tweezers for pyrolysis tubes (bake out for decontamination) and insert the necessary amount of quartz wool with pointed tweezers into the tube.
    2. Insert two steel sticks (bake out for decontamination) at each side of the pyrolysis tube and compress the wool into a 1–2 mm thick stopper. The stopper must be positioned at the lower third of the pyrolysis tube to achieve adequate heating during the pyrolysis process.
    3. Ignite a gas burner....

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结果

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The method includes a two-step chromatographic approach for each sample (Figure 1). In the first run, the sample is dried inside the injector system at 90 °C before volatile compounds are transferred onto the column. Since the drying process is incomplete in most cases, residual solvents and volatile compounds are transferred and analyzed. In the second run, the previously dried sample is subsequently pyrolyzed to facilitate the analysis of non-volatile organ.......

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讨论

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Py-GC-MS is a useful screening method for a broad range of substances in tattoo inks that can also be used for the analysis of other products. Compared to other methods, py-GC-MS can be conducted with only minimal sample preparation. GC-MS devices can be found in most analytical laboratories compared to more specialized methods such as MALDI-ToF-MS and EDX.

The data evaluation of pyrograms may be challenging, since the list of possible ingredients is infinite in theory and library searches tha.......

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披露

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The authors have nothing to disclose.

致谢

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This work was supported by the intramural research project (SFP #1323-103) at the German Federal Institute for Risk Assessment (BfR).

....

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材料

本文使用的材料清单
姓名公司目录编号评论
99.999% 氦载气Air Liquide， Dü德国塞尔多夫-
5975C 带三轴检测器的惰性 XL MSD安捷伦科技公司-德国瓦尔德布隆-
7890A 气相色谱仪瓦尔德布隆安捷伦科技公司-
AMDIS 软件（版本 2.7）美国国家标准与技术研究院，美国马里兰州盖瑟斯堡-可用于 GC/MS 峰积分，例如传输到热释图评估软件
Cold Injection System （CIS）Gerstel， Mühlheim， Germany-
电子碰撞 （EI） 源Agilent Technologies， Waldbronn，Germany-Enhanced
ChemStation （E02.02.1431）AgilentTechnologies， Waldbronn，Germany-usedto generate Average Mass Spektra （AMS）， can be used for peak integration and standard GC/MS library search
J&W HP-5MS 气相色谱柱，30 m，0.25 mm，0.25 µm，5975T 色谱柱环形组件Agilent Technologies，Waldbronn，德国29091S-433LTM
MassHunter 软件Agilent Technologies，Waldbronn，德国-未指定版本，可用于 GC/MS 峰积分和标准 GC/MS 数据库搜索
微量毛细管 Drummond 微量胶囊，体积 2 和微量;LSigma-Aldrich， St. Louis， MO， USAP1549-1PAK
MS ChromSearch （Version 4.0.0.11）Axel Semrau GmbH & Co. KG， Sprockhövel，德国专用高温图评估软件
NIST MS 搜索程序（MS 搜索版本 2.0g）美国国家标准与技术研究所，马里兰州盖瑟斯堡-用于 MS 和 AMS 库的生成以及使用自制和商用库进行相应物质搜索
NIST/EPA/NIH 质谱库 （EI） mainlib 和 replib（数据版本：NIST v11）美国国家标准与技术研究院，马里兰州盖瑟斯堡-使用商业质谱库
聚苯乙烯（平均 Mw ~192,000）Sigma-Aldrich，密苏里州圣路易斯，美国430102-1KG
热解管，管型 - 石英玻璃 - 长度 25 mm;100 单位Gerstel，Mühlheim， Germany018131-100-00
用于 TDUGerstel， Mü 的热解器模块;hlheim， 德国-
石英棉Gerstel， Mühlheim， 德国009970-076-00
钢棒Gerstel， Mü德国 hlheim-
热脱附装置 （TDU 2）Gerstel， Mü德国 hlheim-
运输适配器Gerstel， Mühlheim， 德国018276-010-00
热解管用镊子Gerstel， Mühlheim，德国009970-074-00Zebron
Z-Guard 高温保护柱，气相色谱盖柱，10 m x 0.25 mm，EaPhenomenex Ltd. 德国，阿沙芬堡，德国7CG-G000-00-GH0
德国

参考文献

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  1. Dirks, M. Tattooed skin and health. Vol. 48. Current Problems in Dermatology. Serup, J., Kluger, N., Bäumler, W. , Karger. 118-127 (2015).
  2. Engel, E., et al. Establishment of an extraction method for the recovery of tattoo pigments fr....

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