柱前衍生化法测定化学合成丹皮酚中硫酸二甲酯残留量

摘要

Objective To develop a high performance liquid chromatography coupled with pre-column derivatization method for determi-ning dimethyl sulphate ( DMS) in synthetic paeonol samples .Methods The synthetic paeonol samples reacted with p-nitrophenol un-der alkaline and heating conditions and synthesized p-nitroanisole,which was determined by HPLC-UV detector,with C18 (250 mm × 4.6 mm,5 μm) as column.Results The conversion rate of this derivatization was stable and durable .The solvent blank and paeonol samples did not interfere with the determination of DMS .The linear range appeared from 0.122 to 1.120 mg· L-1 .The detection limit was 0.82 ng.The precision measured by relative standard deviation (RSD) of peak area for the standard solution was 1.69%(n=6) for intra-day detection and 1.89%(n=12) for inter-day detection,respectively.The average recovery was 98.8%(RSD=1.40%,n=9) .Conclusions The method is applicable ,specific,and accurate for the determination of DMS in synthetic paeonol samples .%目的：建立一种化学合成丹皮酚中硫酸二甲酯残留的柱前衍生化高效液相色谱测定方法。方法硫酸二甲酯在碱性和加热的条件下与对硝基苯酚反应生成对硝基茴香醚，经C18柱分离，用紫外检测器检测。结果衍生反应转化率稳定，耐用性良好，空白及丹皮酚供试品均不干扰硫酸二甲酯的检测，硫酸二甲酯浓度在0．122～1．220 mg · L-1的范围内具有良好的线性关系，检出限为0．82 ng，对照溶液测定的峰面积日内和日间精密度的相对标准偏差分别为1．69％（n＝6）和1．89％（n＝12），平均加样回收率98．8％（RSD＝1．40％，n＝9）。结论该法专属性高、精密度好、准确灵敏，适用于测定化学合成丹皮酚中的硫酸二甲酯残留。