Wróbel-Zasada K, Wróbel-Kaczmarczyk K, Luis López-de-Alba P, López-Martínez L, Antonio García-López M
Talanta. 1996 Jul;43(7):1055-60. doi: 10.1016/0039-9140(96)01859-0.
The use of an internal standard is proposed in this work for first derivative spectrophotometric determination of azinphos in formulations. Generally, the spectrophotometric procedure is simpler and less expensive than chromatographic techniques recommended for the analysis of pesticides. However, while determining the pesticide in commercial formulations the, many-fold dilution required for such sensitive detection is a serious source of analytical error. It is known that an internal standard (IS), if properly chosen, can help eliminate this type of problem. A mixture of acetophenone (used as an IS in the high performance liquid chromatography (HPLC) procedure) and the blue dye Erioglaucine (A) was applied for the determination of azinphos-methyl in commercial formulations. To ensure the best conditions for the zero-crossing technique, the composition of the mixture was optimized to obtain the zero value of the first derivative absorbance of the IS at a minimum of the azinphos-methyl first derivative absorbance. Also, at the maximum of the first derivative spectrum of the IS, the differential absorption signal of the analyte was negligible. Analytical characteristics for the first derivative spectrophotometric procedure proposed were evaluated (r(2) = 0.9998, detection limit = 0.043 mg, quantification limit = 0.143 mg) and the analytical results obtained (35.02 +/- 0.20% of azinphos-methyl in the formulation) were in good agreement with the results obtained using the official HPLC method (35.44 +/- 0.32%).
本研究提出使用内标物通过一阶导数分光光度法测定制剂中的谷硫磷。一般来说,分光光度法比推荐用于农药分析的色谱技术更简单且成本更低。然而,在测定商业制剂中的农药时,这种灵敏检测所需的多倍稀释是分析误差的一个严重来源。众所周知,如果选择得当,内标物(IS)有助于消除这类问题。苯乙酮(在高效液相色谱(HPLC)法中用作内标物)和蓝色染料亮蓝(A)的混合物被用于测定商业制剂中的甲基谷硫磷。为确保零交叉技术的最佳条件,对混合物的组成进行了优化,以使内标物的一阶导数吸光度在甲基谷硫磷一阶导数吸光度的最小值处为零。此外,在内标物的一阶导数光谱的最大值处,分析物的微分吸收信号可忽略不计。对所提出的一阶导数分光光度法的分析特性进行了评估(r(2) = 0.9998,检测限 = 0.043 mg,定量限 = 0.143 mg),所得分析结果(制剂中甲基谷硫磷含量为35.02 +/- 0.20%)与使用官方HPLC法获得的结果(35.44 +/- 0.32%)高度一致。