时间分辨同步荧光法同时检测水中硫酸新霉素和磺胺二甲基嘧啶含量

为探究同时检测水中的硫酸新霉素(NEO)和磺胺二甲基嘧啶(SM2)的新方法,根据NEO和SM2在2-巯基乙醇的存在下可与邻苯二甲醛生成具有荧光特性的衍生物,建立时间分辨同步荧光法同时检测水中NEO和SM2的含量。通过研究不同组分的时间分辨同步荧光光谱,确定NEO与邻苯二甲醛衍生物、SM2与邻苯二甲醛衍生物的同步激发特征峰分别为335和291 nm波长处,最佳采集时间分别为1和80 min,最佳同步波长差分别为120和150 nm;采用单因素试验考察邻苯二甲醛溶液、2-巯基乙醇溶液和BR缓冲液的加入量对荧光强度的影响,确定最优的加入量:邻苯二甲醛溶液1.0 mL、2-巯基乙醇溶液0.25 mL、BR缓冲液0.025 mL;据此建立NEO浓度与荧光强度的线性关系,在0.5~14.0 mg·L^-1范围内,得到其线性方程为Y=14.73X+6.14;建立SM2浓度与荧光强度的线性关系,在0.25~9.0 mg·L^-1范围内,得到其线性方程为Y=13.86X+21.49。NEO和SM2的检出限分别为0.5和0.25 mg·L^-1,训练集决定系数(RC2)分别为0.997 5和0.966 9,水中NEO和SM2含量的真实值与预测值之间的预测集决定系数(RP2)分别为0.998 2和0.988 9,预测集均方根误差(RMSEP)分别为0.380 3和0.257 5 mg·L^-1,回收率分别处于101.8%~114.0%和92.3%~115.8%之间,相对标准偏差(RSD)分别为4.0%~8.4%和3.6%~6.6%。本方法线性关系良好,可实现水中NEO和SM2的同时测定。

Simultaneous Determination of Neomycin Sulfate and Sulfadimidine in er by Time-resolved Synchronous Fluorescence Spectrometry

In order to explore a new method for the simultaneous determination of neomycin sulfate (NEO) and sulfamethazine (SM2) in water, according to in the presence of 2-mercaptoethanol, derivatives that NEO or SM2 reacted with o-phthalaldehyde to form have fluorescent properties. Based on this, a time-resolved synchronous fluorescence method was developed for the simultaneous determination of NEO and SM2 in water. The time-resolved synchronous fluorescence spectra of different components were studied. The synchronous excitation peaks of derivatives that NEO or SM2 reacted with o-phthalaldehyde to form were 335 and 291 nm, respectively. Their optimum acquisition times were 1 and 80 min with their optimum synchronization wavelength differences of 120 and 150 nm, respectively. The addition amounts of o-phthalaldehyde solution, 2-mercaptoethanol solution and BR buffer on the fluorescence intensities were investigated by using the single factor experiment. Optimum addition amounts were as follows: o-phthalaldehyde solution of 1.0 mL, 2-mercaptoethanol solution of 0.25 mL, and BR buffer of 0.025 mL. On the basis of these conditions, the linear regression equation was established between NEO concentrations and fluorescence intensities and the linear equation was Y=14.73X+6.14 when the concentration range was 0.5~14.0 mg·L^-1. At the same time, the linear regression equation was established between SM2 concentrations and fluorescence intensities and the linear equation was Y=13.86X+21.49 when the concentration range was 0.25~9.0 mg·L^-1. The detection limits of NEO and SM2 were 0.5 and 0.25 mg·L^-1, respectively. The determination coefficient (RC2) were 0.99 75 and 0.966 9 in the training set, respectively. The determination coefficient (RP2) between the true values and predictive values of NEO and SM2 contents in water were 0.998 2 and 0.988 9 in the prediction set, respectively. Their root mean square errors for the prediction set (RMSEP) were 0.380 3 and 0.257 5 mg·L^-1 with the recoveries of 101.8%~114.0% and 92.3%~115.8% as well as the relative standard deviation (RSD) of 4.0%~8.4% and 3.6%~6.6% respectively. The results showed that there was a good linear relationship and the method could achieve simultaneous determination of NEO and SM2 in water.