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建立了同时提取和测定蔬菜中有机酸与磺胺类抗生素的方法。通过对液相色谱分析条件的优化,建立了以Penomenex C18为分析柱,以0.5%(NH_4)_2HPO_4-H_3PO_4溶液(pH 3.0)为流动相,柱温30℃,流速1.0 m L/min,紫外检测器检测波长为210 nm和270 nm的检测方法。并比较了水提取,0.1%H_3PO_4,0.5%(NH_4)HPO_4,0.5%KH_2PO_44种不同溶液对有机酸和磺胺的提取效果。结果表明:4种提取方法下,乙酸、柠檬酸提取率无显著性差异,草酸、苹果酸、富马酸、磺胺(SA)、磺胺二甲基嘧啶(SM2)均以水提的效果较好。7种有机酸和2种磺胺类抗生素线性关系良好,检出限为0.21~1.95 ng/g,样品的加标回收率81.2%~96.2%,相对标准偏差(RSD)小于8.6%,方法适用于蔬菜中有机酸和磺胺类抗生素快速、高效的分离。
A method of simultaneous extraction and determination of organic acids and sulfonamides in vegetables was established. A liquid chromatography with Penomenex C18 was developed with 0.5% (NH 4) _2HPO_4-H_3PO_4 solution (pH 3.0) as mobile phase at a flow rate of 1.0 mL / Detector detection wavelength of 210 nm and 270 nm detection methods. The effects of water extraction, 0.1% H_3PO_4, 0.5% (NH_4) HPO_4 and 0.5% KH_2PO_4 on the extraction of organic acids and sulfonamides were compared. The results showed that there was no significant difference in the extraction rate of acetic acid and citric acid between the four extraction methods. The effect of water extraction on oxalic acid, malic acid, fumaric acid, sulfadiazine (SA) and sulfamethazine (SM2) was better . The linear relationship between the seven organic acids and the two sulfonamides was good, with the detection limits of 0.21-1.95 ng / g, the spiked recoveries of samples were 81.2% -96.2% and the relative standard deviations (RSDs) were less than 8.6% Vegetables and sulfonamides in organic acids fast and efficient separation.