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目的建立检测生物检材中百草枯的顶空固相微萃取-气相色谱-质谱联用(HS-SPME-GC/MS)的分析方法。方法尿样中加乙基百草枯作为内标,在氯化镍作催化剂的条件下,用硼氢化钠在碱性条件下进行还原,HS-SPME萃取,提取物经GC/MS分析。全血需先离心,沉淀血细胞提取上清液,再用甲醇沉淀蛋白。最终得到的上清液加内标乙基百草枯,以下操作同尿样。结果尿样和血样中的百草枯的还原产物在1.0μg/mL~100μg/mL范围内线性关系良好,回归方程分别为y=0.0957x-0.0163,r=0.9974(n=6);y=0.1096x+0.0871,r=0.9964(n=6)。尿样、血样低、中、高三个质量浓度,RSD值均小于7%。回收率分别为尿样85.49%~100.83%,血样94.72%~99.68%。结论本法操作简便易行、灵敏度高、快速准确。为检测生物检材中的百草枯提供了有效的方法。
Objective To establish a method for the determination of paraquat in biological samples by headspace solid-phase microextraction-gas chromatography-mass spectrometry (HS-SPME-GC / MS). Methods Ethyl paraquat was used as an internal standard in urine samples. The samples were reduced with sodium borohydride under alkaline conditions and HS-SPME with nickel chloride as catalyst. The extracts were analyzed by GC / MS. Whole blood should be centrifuged, the supernatant was precipitated from blood cells, and the protein was precipitated with methanol. The final supernatant plus standard ethyl paraquat, the following operation with the urine sample. Results The calibration curves of paraquat in urine samples and blood samples showed good linearity in the range of 1.0μg / mL ~ 100μg / mL with regression equations of y = 0.0957x-0.0163, r = 0.9974 (n = 6) x + 0.0871, r = 0.9964 (n = 6). Urine samples, blood samples were low, medium and high concentrations of three concentrations, RSD values were less than 7%. The recoveries were 85.49% to 100.83% for urine samples and 94.72% to 99.68% for blood samples. Conclusion This method is easy to operate, high sensitivity, fast and accurate. It provides an effective method for the detection of paraquat in biological samples.