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    尼龙膜富集-可见漫反射光谱法测定人参中乙酰甲胺磷

    Determination of Acephate in Ginseng by Visible Diffuse Reflectance Spectroscopy with Enrichment on Nylon Membrane

    • 摘要: 取人参粉末样品约1 g,用7 mL丙酮超声提取10 min,提取液过滤后蒸缩至1.0 mL,加入4 mL水,1 mL硫酸,40 g·L-1过硫酸钾溶液5 mL,小火煮沸近30 min,并保持溶液体积在25~30 mL之间。冷却后,用100 g·L-1氢氧化钠溶液调节pH至5~8,将溶液移入50 mL容量瓶中,加入26 g·L-1钼酸铵溶液2.0 mL,100 g·L-1抗坏血酸溶液1.0 mL,加水至刻度,静置10 min。取此溶液5.0 mL,在0.07 MPa真空度下使溶液抽滤流经尼龙膜,使所生成的钼蓝吸附在尼龙膜上。抽滤结束时,取出滤膜,风干后,用可见漫反射光谱仪采集滤膜上钼蓝的可见漫反射光谱。试验测得乙酰甲胺磷(AMP)的质量浓度在0.5~5.0 mg·L-1内与其对应的膜漫反射吸光度呈线性关系,其检出限(3s)为0.18 mg·L-1。按所提出方法以空白人参样品为基体加入AMP标准溶液进行回收试验,测得回收率为94.0%~104%,测定值的相对标准偏差(n=5)为1.4%~5.7%。

       

      Abstract: Powdered ginseng sample (about 1 g) was extracted ultrasonically with 7 mL of acetone for 10 min, and the extract was separated and concentrated to a volume of 1.0 mL. 4 mL of water, 1 mL of H2SO4 and 5 mL of 40 g·L-1 K2S2O8 solution were added, and the solution was heated to incipient boiling for 30 min, while keeping its volume between 25 to 30 mL. After cooling, acidity of the solution was adjusted to pH 5-8 with 100 g·L-1 NaOH solution. The solution was transferred to a 50 mL volumeric flask, and 2.0 mL of 26 g·L-1 ammonium molybdate solution and 1.0 mL of 100 g·L-1 ascorbic acid solution were added and diluted to 50.0 mL with water. Let the solution to stand for 10 min. 5.0 mL of the solution were taken and filtered through nylon membrane by suction at a pressure of 0.07 MPa, during the process of which the "Mo blue" was adsorbed on the membrane. At the end of filtration, the membrane was taken and dried in air, and then the reflection absorbance of "Mo blue" on the membrane was measured by visible-diffuse reflectance spectrometer. It was shown that linear relationship between values of reflection absorbance and respective mass concentrations of acephate was obtained in the range of 0.5 to 5.0 mg·L-1 with detection limit (3s) of 0.18 mg·L-1. Using blank ginseng sample as matrix, recovery was tested by standard addition method, giving results of recovery in the range of 94.0% to 104%, and values of RSDs (n=5) found were in the range of 1.4% to 5.7%.

       

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