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采用自动顶空固相微萃取-气相色谱/质谱联用技术,建立了一种快速测定水中7种腥味醛类物质的方法,重点针对纤维萃取头类型、萃取方式、萃取温度、萃取时间以及离子强度等影响因素进行了优化。自动固相微萃取优化后条件为:CAR/PDMS(85μm)纤维头,Na Cl含量25%(W/V),65℃恒温振荡10 min,顶空萃取20 min,250℃下解吸3 min进入气相色谱/质谱进行分析。在优化的前处理和分析条件下,7种物质的回收率为86.30%~113.61%,方法检出限为1.61~17.53 ng/L,远低于各种物质的嗅阈值。
A rapid headspace solid phase microextraction-gas chromatography-mass spectrometry (GC-MS / MS) technique was developed for the rapid determination of seven kinds of fishy aldehydes in water. The methods of fiber extraction heads, extraction methods, extraction temperature, extraction time and Ionic strength and other factors were optimized. The optimum conditions of auto-SPME were: CAR / PDMS (85μm) fiber head, 25% (W / V) NaCl content, shaking at 65 ℃ for 10 min, headspace extraction for 20 min and desorption at 250 ℃ for 3 min Gas chromatography / mass spectrometry analysis. Under optimized conditions of pretreatment and analysis, the recoveries of seven substances ranged from 86.30% to 113.61%. The detection limits were 1.61-17.53 ng / L, far lower than the olfactory thresholds of various substances.