Skoulika S G, Georgiou C A, Polissiou M G
Chemistry Laboratory, Agricultural University of Athens, 75 Iera Odos, 11855 Athens, Greece.
Talanta. 2000 Mar 6;51(3):599-604. doi: 10.1016/s0039-9140(99)00336-7.
FT-Raman spectroscopy based on band intensity and band area measurements, was used for the quantitative determination of diazinon in pesticide formulations. Bands at 554, 604, 631, 1562 and 2971 cm(-1) were used for calibration. Spectra were acquired by averaging 100 scans at a resolution of 4 cm(-1). Calibration curves were linear (correlation coefficients, 0.992-0.9992 and 0.99-0.999 for band intensity and band area measurements, respectively) in the range of 0.2-3.5 M for 554 and 2971 cm(-1), 0.3-3.5 M for 604 cm(-1), 0.6-3.5 M for 1562 cm(-1) and 1.0-3.5 M for 631 cm(-1) bands. Normalization of calibration curves against the 802 cm(-1) cyclohexane band improved their long term stability and minimized the effect of laser beam power fluctuations. No interference was found by commonly used surfactants and the proposed method was applied to the analysis of diazinon formulations. Results obtained compare well as indicated by the t-test, with those obtained by the HPLC reference method. Precision ranged between 0.2-7.8 and 0.1-7.2% RSD, (n=4) for band intensity and band area measurements, respectively. The proposed method is rapid, simple and safe, as toxic samples are analyzed 'as received' without sample pre-treatment, permiting the routine analysis of pesticides formulations.
基于谱带强度和谱带面积测量的傅里叶变换拉曼光谱法被用于农药制剂中二嗪农的定量测定。使用554、604、631、1562和2971 cm⁻¹处的谱带来进行校准。光谱通过在4 cm⁻¹的分辨率下平均100次扫描获得。校准曲线在554和2971 cm⁻¹处0.2 - 3.5 M范围内、604 cm⁻¹处0.3 - 3.5 M范围内、1562 cm⁻¹处0.6 - 3.5 M范围内以及631 cm⁻¹处1.0 - 3.5 M范围内呈线性(谱带强度和谱带面积测量的相关系数分别为0.992 - 0.9992和0.99 - 0.999)。以802 cm⁻¹环己烷谱带对校准曲线进行归一化处理提高了其长期稳定性,并使激光束功率波动的影响最小化。未发现常用表面活性剂有干扰,所提出的方法被应用于二嗪农制剂的分析。t检验表明,所得结果与高效液相色谱参考方法所得结果相比良好。谱带强度和谱带面积测量的精密度分别为0.2 - 7.8%和0.1 - 7.2%相对标准偏差(n = 4)。所提出的方法快速、简单且安全,因为有毒样品无需样品预处理即可“原样”分析,允许对农药制剂进行常规分析。