出 处:《化学分析计量》2023年第7期109-116,共8页Chemical Analysis And Meterage
摘 要:安全套证据的分析通常集中于检测避孕套表面的硅基润滑剂,如聚二甲基硅氧烷(PDMS),以及少量其它润滑剂如甘油,丙二醇等,有时还会对安全套上的其它功能成分聚乙二醇(PEG)、壬苯醇醚-9等和固体颗粒进行检验。从样品制备、显微镜分析、光谱分析、色谱分析、质谱分析五个方面概述了PDMS、PEG和壬苯醇醚-9等物质的有效检测方法。光学显微镜和扫描电镜通常用于分析避孕套表面的固体颗粒;傅里叶变换红外光谱则用于分析PDMS和PEG,其可以识别样品吸收峰的相对丰度,但缺乏具体的识别能力,主要用作筛选方法;拉曼光谱主要用于分析PDMS、PEG、壬苯醇醚-9;核磁共振可以用于分析PDMS、PEG、壬苯醇醚-9,具有很高的灵敏度和区分能力;气相色谱-质谱(GC-MS)可以检测PDMS、PEG、壬苯醇醚-9,但由于目标物所需挥发温度普遍高于仪器承受范围,以及毛细管柱中含有被检测物PDMS,导致无法辨别柱流失导致的假阳性,难以成为主流方法;热解气相色谱-质谱(Py-GC/MS)尤其适合用于检测PDMS,其将PDMS进行裂解,对其裂解后的产物进行检测,不会出现柱流失导致的假阳性并且能够分析检测物聚合度;液相色谱(LC)适用于GC无法分析的分子非挥发性化合物如壬苯醇醚-9;电喷雾电离(ESI)通常用于检测壬苯醇醚-9和PDMS。无论是单独使用还是与凝胶渗透色谱耦合,ESI都具有良好分辨样品的能力。其能够确定分子是环状还是线性形式,从而确认Py-GC-MS获得的结果,但在检测质量超过4000 Da的化合物时,离子抑制效应会使这些化合物难以检测;基质辅助激光解吸电离可以用于PDMS、PEG的定性和定量分析。结合飞行时间-MS进行检测,是目前这类分析的理想方法。其能够检测大摩尔质量的物质,但无法检测是否存在环状低聚物。该方法比ESI更稳定,可重复性更强。但该方法获得的光谱很复杂,因此很难检测到微�The analysis of condom evidence usually focused on the detection of silicone-based lubricants on the surface of condoms,such as polydimethylsiloxane(PDMS),as well as small amounts of other lubricants such as glycerin,propylene glycol,etc.,and sometimes other functional components polyethylene glycol(PEG),nonoxynol ether-9,etc.and solid particles on the condom.The effective detection methods of PDMS,PEG and nonoxynol ether-9 were summarized from the five perspectives of sample preparation,microscopy analysis,spectroscopic analysis,chromatographic analysis and mass spectrometry analysis.Light microscopy and scanning electron microscopy were commonly used to analyze solid particles on the surface of condoms;Fourier transform infrared spectroscopy was used to analyze PDMS and PEG,which could identified the relative abundance of sample absorption peaks,but lacks specific identification capabilities,and was mainly used as a screening method.Raman spectroscopy was mainly used for the analysis of PDMS,PEG,nonoxynol ether-9;Nuclear magnetic resonance could be used to analyze PDMS,PEG,nonoxynol ether-9 with high sensitivity and discrimination;Gas chromatography-mass spectrometry(GC-MS)could detect PDMS,PEG,nonoxynol ether-9,but due to the volatilization temperature required by the detected substance was generally higher than the instrument tolerance range and the capillary column contains the detected substance PDMS,resulting in the inability to distinguish the false positives caused by column loss,it had not become the mainstream method;Pyrolysis gas chromatography-mass spectrometry(Py-GC/MS)was particularly suitable for the detection of PDMS,which lysed PDMS,detected the product after its cleavage,did not produce false positives caused by column loss,and could analyzed the polymerization degree of the detection object;Liquid chromatography(LC)was suitable for molecules of non-volatile compounds such as nonoxynol ether-9 that could not be analyzed by GC;Electrospray ionization(ESI)was commonly used to detect nonoxynol eth
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