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取(1.42±0.01)g的试样5粒,溶解在5 mol·L-1氢氧化钠溶液8 mL和含内标的正己烷40 mL中,磁力搅拌110 min,静置20 min。取上层萃取液2 mL,用无水硫酸钠干燥,过0.22μm有机相滤膜。所得溶液采用DB-5MS色谱柱进行气相色谱分离。质谱分析采用选择离子监测模式。烟碱的线性范围为4.00~200 mg·L-1,检出限(3s)为0.19 mg·L-1。按标准加入法进行回收试验,回收率在91.0%~96.1%之间,测定值的相对标准偏差(n=6)均小于3.0%。
Five samples of (1.42 ± 0.01) g were dissolved in 8 mL of 5 mol·L-1 sodium hydroxide solution and 40 mL of n-hexane containing internal standard. The mixture was magnetically stirred for 110 min and allowed to stand for 20 min. Take the upper extract 2mL, dried over anhydrous sodium sulfate, 0.22μm organic phase filter. The resulting solution was chromatographed on a DB-5MS column. Mass spectrometry analysis using selected ion monitoring mode. The linear range of nicotine was 4.00 ~ 200 mg · L-1, and the limit of detection (3s) was 0.19 mg · L-1. According to the standard addition method, the recoveries were between 91.0% and 96.1%. The relative standard deviations (n = 6) of the measured values were less than 3.0%.