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Simple analysis of naphthalene in human whole blood and urine by headspace capillary gas chromatography with large-volume injection

机译:顶空毛细管气相色谱-大体积进样简单分析人全血和尿中的萘

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摘要

A very simple method for analysis of naphthalene in human whole blood and urine by headspace gas chromatography (GC) is presented. It does not require solid-phase microextraction or cryogenic trapping devices, but needs only a conventional capillary GC instrument with flame ionization detection. The advantage of the method is that as much as 5 ml of headspace vapor can be injected into a GC instrument in splitless mode for sensitive detection. After heating a diluted whole blood or urine sample containing naphthalene and 1-methylnaphthalene (internal standard, IS) in a 7.0-ml vial at 80°C for 30 min, 5 ml of the headspace vapor was drawn with a glass syringe and injected into the gas chromatograph. Before injection, the column temperature was set at 50°C to trap the analytes, and then the oven temperature was programmed up to 300°C. Sharp peaks were obtained for both analyte and IS, and only a few impurity peaks appeared, which did not interfere with the test peaks, mainly for whole blood samples. The detection limit (signal-to-noise ratio. 3) were about 0.05 and 0.01 μg/ml for whole blood and urine, respectively. Precision and linearity were also examined to confirm the reliability. Such a simple headspace GC technique with large-volume injection will be applicable to other low-volatility compounds in biological matrices, and will be useful in forensic toxicological analysis.
机译:提出了一种通过顶空气相色谱法(GC)分析人全血和尿液中萘的非常简单的方法。它不需要固相微萃取或低温捕集装置,而仅需要具有火焰电离检测功能的常规毛细管气相色谱仪。该方法的优势在于,可以不分流模式将多达5 ml的顶空蒸气注入GC仪器中,以进行灵敏的检测。将稀释后的含有萘和1-甲基萘(内标,IS)的全血或尿液样品在7.0 ml小瓶中于80°C加热30分钟后,用玻璃注射器抽出5 ml顶空蒸气并注入气相色谱仪进样前,将柱温设置为50°C以捕获分析物,然后将柱箱温度设置为300°C。对于分析物和IS均获得了尖锐的峰,并且仅出现了少数杂质峰,这并不干扰测试峰,主要是针对全血样品。全血和尿液的检出限(信噪比3)分别约为0.05和0.01μg/ ml。还检查了精度和线性度以确认可靠性。这种具有大体积进样的简单顶空GC技术将适用于生物基质中的其他低挥发性化合物,并将用于法医毒理分析。

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