荧光衍生法测定4种中药饮片SO_(2)残留量研究

Determination of SO_(2) Residues in Four Kinds of Chinese Medicine Decoction Pieces by Fluorescence Derivation Method

目的采用衍生化反应,建立荧光分光光度法测定山药、党参、黄芪、当归中二氧化硫(SO2)残留量。方法通过查阅文献,确定在磷酸氢二钠-磷酸二氢钾缓冲溶液pH为6.4,用量为5.0 mL;1.0 mmol/L邻苯二甲醛溶液2.5 mL;5.0 mmol/L乙酸铵溶液1.5 mL;静置反应时间为40 min的荧光衍生条件下,在激发波长321 nm、发射波长384 nm处测定荧光强度。结果荧光强度与亚硫酸钠标准品浓度在0.2013~402.5696μmol/L线性关系良好,r=0.9999,平均回收率为97.1%,RSD为1.1%。结论测定中药材SO2残留量,采用荧光衍生法灵敏度高,可为山药、党参、黄芪、当归中SO_(2)残留量的测定提供参考,具有简便易行、快速准确等特点,其自动化程度高,适用于基层医院大批量样品提取,提高检测效率,从而保障药品质量。

Objective To establish a fluorescence spectrophotometric method for the determination of SO2 residues in Shanyao(Dioscoreae Rhizoma),Dangshen(Codonopsis Radix),Huangqi(Astragali Radix),Danggui(Angelicae Sinensis Radix).Methods By consulting literature review,the fluorescence derivation condition was determind:the buffer solution of disodium hydrogen phosphate/potassium dihydrogen phosphate(pH 6.4)was 5.0 mL,1.0 mmol/L phthalaldehyde solution was 2.5 mL,and 5.0 mmol/L ammonium acetate solution was 1.5 mL,the standing reaction time was 40 min.The fluorescence intensity at the excitation wavelength of 321 nm and emission wavelength of 384 nm was measured under the above fluorescence derivation conditions.Results The linear relationship between the fluorescence intensity and the concentration of sodium sulfite was 0.2013-402.5696μmol/L(R=0.9999).The average recovery was 97.1%with RSD of 1.1%.Conclusion The fluorescence derivatization method has high sensitivity in the determination of sulfur dioxide residues in Chinese medicinal materials,which could provide reference for the determination of SO^(2) residues in Shanyao(Dioscoreae Rhizoma),Dangshen(Codonopsis Radix),Huangqi(Astragali Radix),Danggui(Angelicae Sinensis Radix).It has the characteristics of simple,easy,rapid and accurate,and has a high degree of automation.It is suitable for the extraction of large quantities of samples in basic hospitals to improve the detection efficiency,so as to ensure the quality of drugs.