矫味型口服补液盐散(Ⅲ)中5-羟甲基糠醛的限量检查

Limit test for 5-hydroxymethylfurfural in flavored oral rehydration salts(Ⅲ)

目的建立矫味型口服补液盐散(Ⅲ)中5-羟甲基糠醛的高效液相色谱分析方法。方法以鸟苷为内标,10%甲醇为提取溶液,建立了HPLC法进行5-羟甲基糠醛限量检测的方法。采用十八烷基硅胶色谱柱,UV检测器,5-羟甲基糠醛检测波长为284 nm,内标物鸟苷检测波长为254 nm,以0.1%甲酸水溶液和乙腈为流动相梯度洗脱,流速为1.0 mL·min^(-1)。结果本方法能在25 min内完成目标化合物的分离分析。5-羟甲基糠醛在0.019 27~3.192μg·mL^(-1)与峰面积线性关系良好且R2为1.0000;鸟苷在0.000 039 85~0.2266 mg·mL^(-1)与峰面积线性关系良好且R2为0.9993。鸟苷定量限为39.85ng·mL^(-1),5-羟甲基糠醛定量限为19.27 ng·mL^(-1),5-羟甲基糠醛回收率为95.5%,能够满足样品测定的要求。结论该方法简便、准确、可靠,重复性好,可用于矫味型口服补液盐散(Ⅲ)中5-羟甲基糠醛的定量分析和质量控制。

Objective To establish an HPLC method for the analysis of 5-hydroxymethylfurfural in flavored oral rehydration salts powder （Ⅲ）. Methods With guanosine as the intemal standard and 10% methanol as the extraction solution, an HPLC method was established to determine 5-hydroxymethyl furfural. The determination conditions were as follows： C18 column, UV detector, 5-hydroxymethyl furfural detection wavelength at 284 nm, guanosine detection wavelength at 254 nm, 0.1% formic acid aqueous solution and acetonitrile as the mobile phase with gradient elution, and the flow rate at 1.0 mL·min^-1. Results The separation and analysis of the target compound were accomplished within 25 min. The 5-HMF standard had a good linearity at 0.019 27-3.192μg·mL^-1 with R2 = 1.0000; the guanosine standard had a good linearity at 0.000 039 85--0.2266 mg·mL^-1 with R： = 0.9993. The limit of quantitation of guanosine was 39.85 ng·mL^-1, and that of 5-HMF was 19.27 ng·mL^-1. The average recovery was 95.5%, meeting the requirements of sample determination. Conclusion The proposed method is fast, accurate, sensitive and repeatable, which is suitable for the quality control and quantitative analysis of 5-hydroxymethylfurfural.