Name: a two-step pyrolysis-gas chromatography method with mass spectrometric detection for identification of tattoo ink ingredients and counterfeit products
Uploaded: 2019-05-22T15:00:00
Description: Watch this Scientific Journal Video about A Two-Step Pyrolysis-Gas Chromatography Method with Mass Spectrometric Detection for Identification of Tattoo Ink Ingredients and Counterfeit Products at JoVE

这项工作得到了德国联邦风险评估研究所校内研究项目 (BFR #1323-103) 的支持。

1. 纹身油墨制备及样品安装
<ol><li>使用25毫米中空玻璃热解管作为样品架和石英羊毛进行样品制备。<ol>
<li>用专门的热解管的推拿器 (烘焙去污) 抓住热解管, 并将必要数量的石英羊毛与尖推子插入管中。</li>
		<li>在热解管的每一侧插入两根钢棒 (烤出去污), 并将羊毛压缩到1-2 毫米厚的塞子中。塞子必须放置在热解管的下三分之一, 以便在热解过程中实现足够的加热。</li>
		<li>点燃燃气燃烧器, 烤?...

<ol>
	<li>Dirks, M., Serup, J., Kluger, N., B&#228;umler, W. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Tattooed skin and health. Vol. 48. Current Problems in Dermatology. , 118-127 (2015).</li><li>Engel, E., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Establishment+of+an+extraction+method+for+the+recovery+of+tattoo+pigments+from+human+skin+using+HPLC+diode+array+detector+technology.">Establishment of an extraction method for the recovery of tattoo pigments from human skin using HPLC diode array detector technology.</a> Analytical Chemistry. 78 (15), 6440-6447 (2006).</li><li>Poon, K. W. C., Dadour, I. R., McKinley, A. J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=In+situ+chemical+analysis+of+modern+organic+tattooing+inks+and+pigments+by+micro-Raman+spectroscopy.">In situ chemical analysis of modern organic tattooing inks and pigments by micro-Raman spectroscopy.</a> Journal of Raman Spectroscopy. 39 (9), 1227-1237 (2008).</li><li>Timko, A. L., Miller, C. H., Johnson, F. B., Ross, V. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=In+vitro+quantitative+chemical+analysis+of+tattoo+pigments.">In vitro quantitative chemical analysis of tattoo pigments.</a> Archives of Dermatology. 137, 143-147 (2004).</li><li>Boon, J. J., Learner, T. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Analytical+mass+spectrometry+of+artists'+acrylic+emulsion+paints+by+direct+temperature+resolved+mass+spectrometry+and+laser+desorption+ionisation+mass+spectrometry.">Analytical mass spectrometry of artists' acrylic emulsion paints by direct temperature resolved mass spectrometry and laser desorption ionisation mass spectrometry.</a> Journal of Analytical and Applied Pyrolysis. 64, 327-344 (2002).</li><li>Hauri, U. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Inks+for+tattoos+and+permanent+make-up+/+pigments,+preservatives,+aromatic+amines,+polyaromatic+hydrocarbons+and+nitrosamines.">Inks for tattoos and permanent make-up / pigments, preservatives, aromatic amines, polyaromatic hydrocarbons and nitrosamines.</a> Department of Health, Kanton Basel-Stadt. Swiss National Investigation Campaign. , (2014).</li><li>Bocca, B., Sabbioni, E., Mi&#269;eti&#263;, I., Alimonti, A., Petrucci, F. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Size+and+metal+composition+characterization+of+nano-+and+microparticles+in+tattoo+inks+by+a+combination+of+analytical+techniques.">Size and metal composition characterization of nano- and microparticles in tattoo inks by a combination of analytical techniques.</a> Journal of Analytical Atomic Spectrometry. 32 (3), 616-628 (2017).</li><li>Schreiver, I., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Synchrotron-based+nano-XRF+mapping+and+micro-FTIR+microscopy+enable+to+look+into+the+fate+and+effects+of+tattoo+pigments+in+human+skin.">Synchrotron-based nano-XRF mapping and micro-FTIR microscopy enable to look into the fate and effects of tattoo pigments in human skin.</a> Scientific Reports. 7, 11395 (2017).</li><li>Taylor, C. R., Anderson, R. R., Gange, R. W., Michaud, N. A., Flotte, T. J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Light+and+electron+microscopic+analysis+of+tattoos+treated+by+Q-switched+ruby+laser.">Light and electron microscopic analysis of tattoos treated by Q-switched ruby laser.</a> Journal of Investigative Dermatology. 97, 131-136 (1991).</li><li>Namduri, H., Nasrazadani, S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Quantitative+analysis+of+iron+oxides+using+Fourier+transform+infrared+spectrophotometry.">Quantitative analysis of iron oxides using Fourier transform infrared spectrophotometry.</a> Corrosion Science. 50 (9), 2493-2497 (2008).</li><li>Burgio, L., Clark, R. J., Hark, R. R. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Raman+microscopy+and+x-ray+fluorescence+analysis+of+pigments+on+medieval+and+Renaissance+Italian+manuscript+cuttings.">Raman microscopy and x-ray fluorescence analysis of pigments on medieval and Renaissance Italian manuscript cuttings.</a> Proceedings of the National Academy of Sciences of the United States of America. 107 (13), 5726-5731 (2010).</li><li>Manso, M., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Assessment+of+toxic+metals+and+hazardous+substances+in+tattoo+inks+using+Sy-XRF,+AAS+and+Raman+spectroscopy.">Assessment of toxic metals and hazardous substances in tattoo inks using Sy-XRF, AAS and Raman spectroscopy.</a> Biological Trace Element Research. 187 (2), 596-601 (2017).</li><li>Yakes, B. J., Michael, T. J., Perez-Gonzalez, M., Harp, B. P. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Investigation+of+tattoo+pigments+by+Raman+spectroscopy.">Investigation of tattoo pigments by Raman spectroscopy.</a> Journal of Raman Spectroscopy. 48 (5), 736-743 (2017).</li><li>Yang, S. -. H., Shen, J. Y., Chang, M. S., Wu, G. J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Differentiation+of+vehicle+top+coating+paints+using+pyrolysis-gas+chromatography/mass+spectrometry+and+multivariate+chemometrics+with+statistical+comparisons.">Differentiation of vehicle top coating paints using pyrolysis-gas chromatography/mass spectrometry and multivariate chemometrics with statistical comparisons.</a> Analytical Methods. 7, 1527-1534 (2015).</li><li>Schreiver, I., Hutzler, C., Luch, A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Data+from:+Two-step+pyrolysis-gas+chromatography+method+with+mass+spectrometric+detection+for+identification+of+tattoo+ink+ingredients+and+counterfeit+products.">Data from: Two-step pyrolysis-gas chromatography method with mass spectrometric detection for identification of tattoo ink ingredients and counterfeit products.</a> Dryad Digital Repository. , (2019).</li><li>Schreiver, I., Hutzler, C., Andree, S., Laux, P., Luch, A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Identification+and+hazard+prediction+of+tattoo+pigments+by+means+of+pyrolysis&#8212;gas+chromatography/mass+spectrometry.">Identification and hazard prediction of tattoo pigments by means of pyrolysis&#8212;gas chromatography/mass spectrometry.</a> Archives of Toxicology. 90 (7), 1639-1650 (2016).</li><li>Ghelardi, E., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Py-GC/MS+applied+to+the+analysis+of+synthetic+organic+pigments:+characterization+and+identification+in+paint+samples.">Py-GC/MS applied to the analysis of synthetic organic pigments: characterization and identification in paint samples.</a> Analytical and Bioanalytical Chemistry. 407 (5), 1415-1431 (2015).</li><li>Russell, J., Singer, B. W., Perry, J. J., Bacon, A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=The+identification+of+synthetic+organic+pigments+in+modern+paints+and+modern+paintings+using+pyrolysis-gas+chromatography-mass+spectrometry.">The identification of synthetic organic pigments in modern paints and modern paintings using pyrolysis-gas chromatography-mass spectrometry.</a> Analytical and Bioanalytical Chemistry. 400 (5), 1473-1491 (2011).</li><li>Silva, M. F., Domenech-Carbo, M. T., Fuster-Lopez, L., Mecklenburg, M. F., Martin-Rey, S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Identification+of+additives+in+poly(vinylacetate)+artist's+paints+using+PY-GC-MS.">Identification of additives in poly(vinylacetate) artist's paints using PY-GC-MS.</a> Analytical and Bioanalytical Chemistry. 397 (1), 357-367 (2010).</li><li>Peris-Vincente, J., Baumer, U., Stege, H., Lutzenberger, K., Gimeno Adelantado, J. V. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Characterization+of+commercial+synthetic+resins+by+pyrolysis-gas+chromatography/mass+spectrometry:+application+to+modern+art+and+conservation.">Characterization of commercial synthetic resins by pyrolysis-gas chromatography/mass spectrometry: application to modern art and conservation.</a> Analytical Chemistry. 81, 3180-3187 (2009).</li><li>Kleinert, J. C., Weschler, C. J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Pyrolysis+gas+chromatographic-mass+spectrometric+identification+of+polydimethylsiloxanes.">Pyrolysis gas chromatographic-mass spectrometric identification of polydimethylsiloxanes.</a> Analytical Chemistry. 52 (8), 1245-1248 (1980).</li><li>Scalarone, D., Chiantore, O. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Separation+techniques+for+the+analysis+of+artists'+acrylic+emulsion+paints.">Separation techniques for the analysis of artists' acrylic emulsion paints.</a> Journal of Separation Science. 27 (4), 263-274 (2004).</li><li>Sonoda, N. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Characterization+of+organic+azo-pigments+by+pyrolysis-gas+chromatography.">Characterization of organic azo-pigments by pyrolysis-gas chromatography.</a> Studies in Conservation. 44, 195-208 (1999).</li><li>Chiantore, O., Scalarone, D., Learner, T. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Characterization+of+artists'+crylic+emulsion+paints.">Characterization of artists' crylic emulsion paints.</a> International Journal of Polymer Analysis and Characterization. 8 (1), 67-82 (2003).</li><li>Schossler, P., Fortes, I., Figueiredo J&#250;nior, J. C. D., Carazza, F., Souza, L. A. C. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Acrylic+and+Vinyl+Resins+Identification+by+Pyrolysis-Gas+Chromatography/Mass+Spectrometry:+A+Study+of+Cases+in+Modern+Art+Conservation.">Acrylic and Vinyl Resins Identification by Pyrolysis-Gas Chromatography/Mass Spectrometry: A Study of Cases in Modern Art Conservation.</a> Analytical Letters. 46 (12), 1869-1884 (2013).</li><li>Wallisch, K. L. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Pyrolysis+of+random+and+block+copolymers+of+ethyl+acrylate+and+methyl+methacrylate.">Pyrolysis of random and block copolymers of ethyl acrylate and methyl methacrylate.</a> Journal of Applied Polymer Science. 18, 203-222 (1974).</li><li>Hauri, U. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Inks+for+tattoos+and+PMU+(permanent+make-up)+/+Organic+pigments,+preservatives+and+impurities+such+as+primary+aromatic+amines+and+nitrosamines.">Inks for tattoos and PMU (permanent make-up) / Organic pigments, preservatives and impurities such as primary aromatic amines and nitrosamines.</a> State Laboratory of the Canton Basel City. , (2011).</li></ol>

Py-GC-MS 是一种有用的筛选方法, 用于纹身油墨中的各种物质, 也可用于分析其他产品。与其他方法相比, 只有少量的样品制备即可进行 py-GC-MS。与诸如 Aldi-tof-ms 和 EDX 等更专业的方法相比, 大多数分析实验室都可以找到 GC-MS 设备。
热图的数据评估可能具有挑战性, 因为可能的成分列表在理论和图书馆搜索是无限的, 这也解释了物质对母体化合物在图书馆的组合是必要的。这里描?...

纹身油墨是由颜料、溶剂、粘合剂、表面活性剂、增稠剂以及有时还含有防腐剂1的复杂混合物组成的。在过去的几十年里, 纹身的日益普及, 导致整个欧洲制定了解决纹身墨水安全问题的立法。在大多数情况下, 变色颜料及其杂质受到限制, 因此应通过国家实验室市场调查进行监测, 以控制其遵守法律的情况。
利用本文所述的在线热解-气相色谱质谱 (Pyrolysis-gas) 方法, 可以同时识别多种成分。由于挥发性、半挥发性和非挥发性化合物可以在同一过程中分离和分析, 因此与用于纹身油墨分析的其他方法相比, 目标化合物的种类很高。液相色谱方法大多是在有机溶剂中溶解色素的情况下进行的。拉曼光谱以及傅里叶变换红外光谱 (FT-IR) 光谱被认为是识别颜料和聚合物的合适工具, 但由于标准中没有使用分离技术, 因此受到多种成分混合物的限制。实验室应用3,4。激光去光电离-飞行时间质谱 (ldi-tof-ms) 也被用于颜料和聚合物鉴定5,6。总之, 大多数方法缺乏对挥发性化合物的分析。缺乏合适的商业光谱库是所有这些方法的共同缺点。无机颜料的鉴定通常是用电感耦合等离子体质谱 (icp-ms)7、8或能量色散 x 射线光谱 (edx)4,9进行的。此外, ft-ir 和拉曼光谱已被用于分析无机颜料, 如二氧化钛或氧化铁在其他研究领域10,11,12,13。
这项研究的目的是建立一种适用于财务费用适中的标准分析实验室的方法, 以升级现有和常见的设备。这里描述的 Py-GC-MS 是一种非定量的方法, 用于识别混合物中的有机成分。在发现 py-GC-MS 筛选中的可疑物质后, 可以采用更专门的方法对目标物质进行量化。它对于分析非易挥发和不溶性物质 (如颜料和聚合物) 特别有趣。
所述方法可适用于其他应用领域的油墨和清漆。所描述的数据评估方法适用于所有的热解调查。此外, 主要来自亚洲市场的假冒产品对消费者和制造商都表现出潜在的风险来源和经济负担 (2017年在德国雷根斯堡举行的第三 ectp 3号 ectp, 2017年)。这里描述的方法可以用来比较假定的假冒油墨的特点与原来的瓶子, 类似于公布的法医方法的汽车清漆鉴定 14。

<table>
	<tbody>
		<tr>
			<td>99.999% Helium carrier gas</td>
			<td>Air Liquide, D&#252;sseldorf, Germany</td>
			<td>-</td>
			<td></td>
		</tr>
		<tr>
			<td>5975C inert XL MSD with Triple-Axis Detectors</td>
			<td>Agilent Technologies, Waldbronn, Germany</td>
			<td>-</td>
			<td></td>
		</tr>
		<tr>
			<td>7890A gas chromatograph</td>
			<td>Agilent Technologies, Waldbronn, Germany</td>
			<td>-</td>
			<td></td>
		</tr>
		<tr>
			<td>AMDIS software (Version 2.7)</td>
			<td>The National Institute of Standards and Technology, Gaithersburg, MD, USA</td>
			<td>-</td>
			<td>can be used for GC/MS peak integration, e.g. for transfer to pyrogram evaluation software</td>
		</tr>
		<tr>
			<td>Cold Injection System (CIS)</td>
			<td>Gerstel, M&#252;hlheim, Germany</td>
			<td>-</td>
			<td></td>
		</tr>
		<tr>
			<td>electron impact (EI) source</td>
			<td>Agilent Technologies, Waldbronn, Germany</td>
			<td>-</td>
			<td></td>
		</tr>
		<tr>
			<td>Enhanced ChemStation (E02.02.1431)</td>
			<td>Agilent Technologies, Waldbronn, Germany</td>
			<td>-</td>
			<td>used to generate Average Mass Spektra (AMS), can be used for peak integration and standard GC/MS library search</td>
		</tr>
		<tr>
			<td>J&#38;W HP-5MS GC Column, 30 m, 0.25 mm, 0.25 &#181;m, 5975T Column Toroid Assembly</td>
			<td>Agilent Technologies, Waldbronn, Germany</td>
			<td>29091S-433LTM</td>
			<td></td>
		</tr>
		<tr>
			<td>MassHunter Software</td>
			<td>Agilent Technologies, Waldbronn, Germany</td>
			<td>-</td>
			<td>no Version specified, can be used for GC/MS peak integration and standard GC/MS library search</td>
		</tr>
		<tr>
			<td>Microcapillary tube Drummond Microcaps, volume 2 &#181;L</td>
			<td>Sigma-Aldrich, St. Louis, MO, USA</td>
			<td>P1549-1PAK</td>
			<td></td>
		</tr>
		<tr>
			<td>MS ChromSearch (Version 4.0.0.11)</td>
			<td>Axel Semrau GmbH &#38; Co. KG, Sprockh&#246;vel, Germany</td>
			<td>-</td>
			<td>specialized pyrogram evaluation software</td>
		</tr>
		<tr>
			<td>NIST MS Search Program (MS Search version 2.0g)</td>
			<td>The National Institute of Standards and Technology, Gaithersburg, MD, USA</td>
			<td>-</td>
			<td>used for MS and AMS library generation and corresponding substance search with selfmade and commercial libraries</td>
		</tr>
		<tr>
			<td>NIST/EPA/NIH Mass Spectral Library (EI) mainlib &#38; replib (Data version: NIST v11)</td>
			<td>The National Institute of Standards and Technology, Gaithersburg, MD, USA</td>
			<td>-</td>
			<td>used commercial mass spectral library</td>
		</tr>
		<tr>
			<td>Polystyrene (average Mw ~192,000)</td>
			<td>Sigma-Aldrich, St. Louis, MO, USA</td>
			<td>430102-1KG</td>
			<td></td>
		</tr>
		<tr>
			<td>Pyrolysis tubes, tube type - quartz glass - lenght 25 mm; 100 Units</td>
			<td>Gerstel, M&#252;hlheim, Germany</td>
			<td>018131-100-00</td>
			<td></td>
		</tr>
		<tr>
			<td>Pyrolyzer Module for TDU</td>
			<td>Gerstel, M&#252;hlheim, Germany</td>
			<td>-</td>
			<td></td>
		</tr>
		<tr>
			<td>Quartz wool</td>
			<td>Gerstel, M&#252;hlheim, Germany</td>
			<td>009970-076-00</td>
			<td></td>
		</tr>
		<tr>
			<td>Steel sticks</td>
			<td>Gerstel, M&#252;hlheim, Germany</td>
			<td>-</td>
			<td></td>
		</tr>
		<tr>
			<td>Thermal Desorption Unit (TDU 2)</td>
			<td>Gerstel, M&#252;hlheim, Germany</td>
			<td>-</td>
			<td></td>
		</tr>
		<tr>
			<td>Transport adapter</td>
			<td>Gerstel, M&#252;hlheim, Germany</td>
			<td>018276-010-00</td>
			<td></td>
		</tr>
		<tr>
			<td>Tweezers for Pyrolysis tubes</td>
			<td>Gerstel, M&#252;hlheim, Germany</td>
			<td>009970-074-00</td>
			<td></td>
		</tr>
		<tr>
			<td>Zebron Z-Guard Hi-Temp Guard Column, GC Cap. Column 10 m x 0.25 mm, Ea</td>
			<td>Phenomenex Ltd. Deutschland, Aschaffenburg, Germany</td>
			<td>7CG-G000-00-GH0</td>
			<td></td>
		</tr>
	</tbody>
</table>

a two-step pyrolysis-gas chromatography method with mass spectrometric detection for identification of tattoo ink ingredients and counterfeit products

纹身油墨是复杂的成分混合物。它们中的每一个都具有不同的化学性质, 必须在化学分析中加以解决。该方法在首次解吸过程中, 分析了两步热解在线与气相色谱质谱 (py-GC-MS) 挥发性化合物的耦合。在第二次运行中, 对相同的干燥样品进行热解, 以分析非易挥发化合物, 如颜料和聚合物。这些可以通过它们的特定分解模式来识别。此外, 此方法可用于区分原装和假冒油墨。采用平均质谱和自制热解文库进行数据评价的简易筛选方法, 加快了物质识别的速度。利用专门的热解 GS-MS 数据评估软件, 可以对全色谱进行快速、可靠的比较。由于采用 GC-MS 作为分离技术, 该方法仅限于样品解吸时和热解后的挥发性物质。该方法可用于市场控制调查中的快速物质筛选, 因为它不需要样品制备步骤。

该方法包括每个样本的两步色谱方法 (图 1)。在第一次运行时, 样品在90°c 的喷射器系统内干燥, 然后将挥发性化合物转移到色谱柱上。由于干燥过程在大多数情况下是不完整的, 残留溶剂和挥发性化合物的转移和分析。在第二次运行中, 对先前干燥的样品进行了热解, 以便利对非易挥发有机成分进行分析。
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A Two-Step Pyrolysis-Gas Chromatography Method with Mass Spectrometric Detection for Identification of Tattoo Ink Ingredients and Counterfeit Products

一种用于检测纹身油墨成分和假冒产品的两步热解-气相色谱法

该方法采用质谱检测和数据评估协议, 与气相色谱联用两步热解, 可用于纹身油墨的多成分分析和假冒产品的鉴别。

Tattoo inks are complex mixtures of ingredients. Each of them possesses different chemical properties which have to be addressed upon chemical analysis. ...

纹身油墨和其他油墨是成分的复杂混合物。我们的方法提供了一种快速、简单的同时分析多个组件的方法。热解，然后耦合气相色谱与质谱检测允许分析非易失和挥发性化合物连续运行。除了纯分析油墨成分外，此方法还可用于区分原装和假冒产品。一般来说，此方法可用于各种液体样品。数据评估方法也可用于任何其他种类的热解数据。与大多数分析技术一样，热图的数据解释是这种方法的致命弱点。因此，我们提供热图库和单分析光谱，以方便对数据的解释。首先用专用钳子握住25毫米的空心玻璃热解管，用尖钳将所需的石英羊毛插入管中。在热解管的每一侧插入两根钢棒，将羊毛压缩成一到两毫米厚的塞子。塞子必须放置在热解管的下三分之一，以实现热解过程中足够的加热。点燃燃气燃烧器，烘烤热解管，从每侧加注两到三秒钟，以去除污染物。接下来，手动摇动纹身墨水瓶一分钟，以确保均匀性。在墨水中浸入两微升微胶囊尖端，通过填充一半的毛细管来吸吸约一微升墨水。将毛细管插入热解管，用墨水染色石英羊毛塞。必须透明颜色染色，而不向样品添加太多墨水。使用专用钳子，将准备好的热解管连接到用于自动喷射单元的钢制运输适配器上，并检查热解管是否完全垂直，且在摇动过程中不会脱落。将运输适配器放在自动喷射单元的托盘中，使其处于所需的位置，用于热解 GCMS 分析。对于挥发性化合物的数据评估，启动GCMS分析MS库搜索软件，并打开脱吸运行的色谱图。单击"频谱"并选择商业库，然后选择"库"。然后加载感兴趣的库。选择"集成参数"，然后单击"频谱"和"库搜索报告"执行库搜索。对于热解数据评估，打开热解运行的色谱图。在 GCMS 评估软件中标记整个色谱图。使用鼠标右键，按下可获取平均质谱（AMS）。要建立自制库，请单击"频谱"和"编辑库"。选择感兴趣的库，后跟"添加新条目"，然后填写所有感兴趣的信息。生成已调查的墨迹图的 AMS，并使用库搜索与自制的 AMS 库进行比较。排除柱出血或其他柱噪声的群众。要使用专门的热图评估软件识别非易失性化合物，请构建一个包含应用作库的所有热图条目的文件夹，例如颜料识别的颜料图库或原始油墨的图谱，以便将其与假仿制品进行比较。单击"浏览"，在选项卡库搜索中加载未知图。接下来，加载库文件夹，在搜索选项中仅选择 MS 匹配"和 RT 匹配"，因为与参考颜料的图谱相比，总体丰度会有所不同。单击搜索选项中的"高级"。选择感兴趣的 RT 窗口宽度，区域阈值为 0.1%，并允许多个匹配。在"质度规格"选项中，选择参数仅使用具有指定 MS 光谱的峰值，并使用拟合阈值 850。将文件pigment_search_spectra。spf，或单击"添加"，以保存指定的 MS 光谱从参考颜料或聚合物的每个光谱从库的高级搜索选项。按"确定"返回主窗口。然后单击"搜索"以开始比较。如果需要，请转到色谱图匹配选项卡，并在色谱图匹配选项卡下选择化合物。右键单击并选择 NIST 中的搜索频谱"，将频谱转发到 MS 库软件并识别化合物。对于非易失性化合物的手动数据评估，启动GCMS分析MS库搜索软件，并打开热解运行的色谱图。单击"频谱"和"选择库"来选择商业和热解库。加载所有感兴趣的库。将热图集成到 GCMS 评估软件中，并考虑面积不低于总面积 0.2% 的所有峰值。接下来，单击"频谱"和"库搜索报告"启动库搜索。手动比较文本协议中的特定颜料和聚合物分解产物的所有库匹配，或文献中所述的片段。生产精准的油墨具有高纯成分和数量有限的成分，因此色谱图易于用标准库解释，因为大多数峰值都可以识别。但是，即使在高品质的油墨中，除了声明的甘油之外，也经常发现未申报的成分，如丙二醇。含有多种成分和杂质的油墨会导致难以解释的火药。第二次运行中发生的大多数峰值可能不是彼此分离的基线，因此很难进行识别。在数据评估期间，某些物质还可能导致峰值低于阈值集。解释复杂数据的解决方案可能是对同一样本使用 400、600 和 800 摄氏度的连续热解步骤的步进方法。一些颜料分解产物可能来自多种颜料。对于从不同供应商购买的三个柠檬油墨，假冒产品标识的阳性结果证明了这一结果。使用高于0.9的正向匹配系数，将第一次解吸运行的色谱图和原始油墨第二次运行的色谱图与原油墨的三次独立采集进行比较，并使用热图评估软件将两种假冒产品进行比较。热解是有用的，识别多个化合物，只需一个分析方法。特定化合物的鉴定后可以使用更专业的方法进行。

Research

JoVE Journal

Chemistry

Untargeted Metabolomics from Biological Sources Using Ultraperformance Liquid Chromatography-High Resolution Mass Spectrometry (UPLC-HRMS)

Untargeted Metabolomics from Biological Sources Using Ultraperformance Liquid Chromatography-High Resolution Mass Spectrometry UPLC-HRMS

不相关的代谢组学，生物源使用超高效液相色谱 - 高分辨质谱（UPLC-HRMS）

Here we present a workflow to analyze the metabolic profiles for biological samples of interest including; cells, serum, or tissue. The sample is first ...

科研

化学

Mass Spectrometric Approaches to Study Protein Structure and Interactions in Lyophilized Powders

质谱途径研究蛋白质结构和相互作用的冻干粉

Amide hydrogen/deuterium exchange (ssHDX-MS) and side-chain photolytic labeling (ssPL-MS) followed by mass spectrometric analysis can be valuable for ...

Visualization of Ambient Mass Spectrometry with the Use of Schlieren Photography

环境质谱可视化纹影摄影的使用

This manuscript outlines how to visualize mass spectrometry ambient ionization sources using schlieren photography. In order to properly optimize the mass ...

A Straightforward Method for Glucosinolate Extraction and Analysis with High-pressure Liquid Chromatography (HPLC)

A Straightforward Method for Glucosinolate Extraction and Analysis with High-pressure Liquid Chromatography HPLC

简捷方法对硫甙的提取与分析用高压液相色谱法（HPLC）

Glucosinolates are a well-studied and highly diverse class of natural plant compounds. They play important roles in plant resistance, rapeseed oil ...

A Convenient Method for Extraction and Analysis with High-Pressure Liquid Chromatography of Catecholamine Neurotransmitters and Their Metabolites

用高压液相色谱法提取和分析儿茶酚胺神经递质及其代谢物的简便方法

The extraction and analysis of catecholamine neurotransmitters in biological fluids is of great importance in assessing nervous system function and ...

A Two-Step Protocol for Umpolung Functionalization of Ketones Via Enolonium Species

Enolonium 种极性转换酮功能化的两步协议

&#945;-Functionalization of ketones via umpolung of enolates by hypervalent iodine reagents is an important concept in synthetic organic chemistry. ...

Versatile CO2 Transformations into Complex Products: A One-pot Two-step Strategy

Versatile CO2 Transformations into Complex Products: A One-pot Two-step Strategy

多功能 CO2转化为复杂产品：单罐两步战略

CO2 transformations using a one-pot two-step method are presented herein. The purpose of the method is to give access to a variety of value-added products ...

Mass Spectrometry-Guided Genome Mining as a Tool to Uncover Novel Natural Products

质谱导览基因组挖掘作为发现新天然产品的工具

The chemical space covered by natural products is immense and widely unrecognized. Therefore, convenient methodologies to perform wide-ranging evaluation ...

Gas Chromatography-Mass Spectrometry Paired with Total Vaporization Solid-Phase Microextraction as a Forensic Tool

气相色谱-质量光谱学与总蒸发固体相微切成一对，作为取证工具

Gas Chromatography &#8211; Mass Spectrometry (GC-MS) is a frequently used technique for the analysis of numerous analytes of forensic interest, including ...

Radiosynthesis of 1-(2-[18F]Fluoroethyl)-L-Tryptophan using a One-pot, Two-step Protocol

Radiosynthesis of 1-2-[18F]Fluoroethyl-L-Tryptophan using a One-pot, Two-step Protocol

1-（2-[18F]氟乙基）-L-色氨酸的放射性合成，采用一锅两步实验方案

The kynurenine pathway (KP) is a primary route for tryptophan metabolism. Evidence strongly suggests that metabolites of the KP play a vital role in tumor ...