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目的将中空纤维膜-液相微萃取(HF-LPME)与气相色谱-质谱联用技术(GC-MS)相结合,建立血液中氯氮平的高灵敏度检测方法。方法萃取选用聚偏氟乙烯中空纤维,分别优化影响萃取效率的实验条件。血液样品调节至p H=9,以正辛醇为萃取溶剂,于搅拌速率为2 000 r/min条件下中空纤维膜微萃取20 min,取1μl萃取液,采用GCMS分析氯氮平。结果该方法对血液中氯氮平的平均富集因子为20.7。血液中氯氮平浓度在0.01 mg/L~5 mg/L范围内,线性关系良好(r=0.997 3),检出限为0.01 mg/L(S/N=3),加标回收率为92.3%~98.8%,日内精密度<6.2%,日间精密度<8.3%。结论该方法操作简单,所需有机溶剂少,富集效率高,可避免残留和交叉污染,适于血液中氯氮平的检测。
Objective To establish a highly sensitive detection method of clozapine in blood by combining hollow fiber membrane-liquid-phase microextraction (HF-LPME) and gas chromatography-mass spectrometry (GC-MS) Methods Polyvinylidene fluoride hollow fiber was selected for extraction, and the experimental conditions affecting the extraction efficiency were optimized. The blood samples were adjusted to pH = 9, n-octanol was used as the extraction solvent, and the hollow fiber membrane was extracted by micro-extraction for 20 min at a stirring rate of 2000 r / min. 1 μl of the extract was extracted and the clozapine was analyzed by GCMS. Results The average enrichment factor for clozapine in blood was 20.7. The linearity of clozapine in the blood ranged from 0.01 mg / L to 5 mg / L (r = 0.997 3). The detection limit was 0.01 mg / L (S / N = 3) 92.3% ~ 98.8%, intraday precision <6.2%, intraday precision <8.3%. Conclusion The method is simple and requires less organic solvents, high enrichment efficiency, can avoid residue and cross-contamination, suitable for the detection of clozapine in the blood.