摘要
取剪成小片(5mm×5mm)的样品(1.00g),于模拟汗液50mL中,在50℃振荡浸泡2h,冷却至室温,调节其酸度为pH8.0。用微量进样器移取氯苯萃取剂2.0μL,将进样器针尖置于浸泡液液面下方1cm左右处并形成微液滴;在25℃和200r·min^-1的搅拌速率下萃取30min。回收全部萃取液并用甲醇稀释至50μL作为样品溶液。按所选仪器工作条件进行气相色谱-质谱分析。8种抗菌剂的质量浓度均在1.O-40mg·L^-1范围内与其峰面积呈线性关系,方法的检出限(3S/N)在0.08-0.24mg·L^-1之间。以空白样品为基体进行加标回收试验,所得回收率在83.6%-98.99/6之间,测定值的相对标准偏差(n=6)在3.7%-9.1%之间。
A portion of the sliced strip-sample (5 mm×5 ram, 1.00 g) was extracted by shaking with 50 mL of the simulated perspiration at 50℃ for 2 h. After cooling to room temperature, the acidity of the extract was adjusted to pH 8. 0. 2. 0 μL of the extractant-chlorobenzene were added into the perspiration extract using a microsampler with its syringe needle placed 1 cm below the solution surface level, and thence to form a microdroplet, and micro-extraction was performed by agitation at a rate of 200 r·min 1 for 30 rain at 25℃. Whole of the chlorobenzene extract was recovered and diluted to 50μL with methanol for use as sample solution in the following GC-MS analysis under prescribed conditions. Linear relationships between values of peak area and mass concentration of the 8 antibacterial agents were kept in the same range of 1.0-40 mg·L^-1 , with detection limits (3S/N) in the range of 0. 08-0. 24 mg·L^-1. On the base of blank sample, test for recovery was made by standard addition method; values of recovery found were in the range of 83.60%-98.9%, with RSDs (n=6) in the range of 3.7%-9.1%.
出处
《理化检验(化学分册)》
CAS
CSCD
北大核心
2016年第12期1375-1379,共5页
Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
基金
国家质量监督检验检疫总局科技计划项目(2014QK209)