全血中12种挥发性有机物的固相微萃取-气相色谱-质谱-同位素内标测定法

Determination of 12 volatile organic compounds in whole blood by solid phase microextraction-gas chromatography-mass spectrometry-isotope internal standard

目的建立全血中12种挥发性有机物(VOCs)的固相微萃取-气相色谱(GC)-质谱(MS)-同位素内标测定法。方法将血样倒入棕色进样瓶中,将85μm CAR/PDMS纤维插入振荡器中,350 r/min振荡,40℃萃取25 min,300℃解析进样0.5 min,采用GC-MS检测12种挥发性有机物的含量。结果在0.090~5.76 ng/ml的线性范围内,所得12种VOCs的回归方程均呈较好的线性关系(r≥0.996)。该方法的检出限0.03~0.076 ng/ml,定量下限0.053~0.251 ng/ml,平均回收率为84.4%~121.9%,RSD为1.7%~12.5%。结论该方法灵敏度高,操作步骤简单,适合人群血液中挥发性有机物的监测。

Objective To establish a solid phase microextraction gas chromatography（GC）-mass spectrometry（MS）-isotope internal standard method for the determination of 12 volatile organic compounds（VOCs） in whole blood. Methods The blood samples were poured into a brown syringe. 85 μm CAR/PDMS fiber was inserted into the shaker,shaken at 350 r/min,extracted at 40 ℃ for 25 min and analyzed at 300 ℃ for 0.5 min. GC-MS was used to detect 12 volatile organic compounds. Results The method presented a good linearity range（0.090-5.76 ng/ml,r≥0.996）. The limits of detection were 0.03-0.076 ng/ml,the limits of quantification were 0.053-0.251 ng/ml. The spiked recoveries ranged from 84.4% to 121.9% and the relative standard deviations ranged from 1.7% to 12.5%. Conclusion The proposed method is accurate,sensitive and applicable to the rapid analysis of VOCs in the blood samples.