摘要
建立高效液相色谱法同时测定阿胶糕中苯甲酸、山梨酸、脱氢乙酸、水杨酸、苯氧异丙醇、2,6-二氯苯甲醇、苯甲酸甲酯、碘丙炔醇丁基氨甲酸酯、对氯间甲酚、2,4-二氯苯甲醇、σ-伞花烃-5-醇、氯二甲酚、氯咪巴唑、苄氯酚、三氯卡班和硫柳汞钠16种防腐剂的分析方法。阿胶糕经提取、除蛋白质等处理后,采用Kromasil C_(18)色谱柱(250 mm×4.6 mm,5μm)分离,以0.025 mol/L磷酸二氢钠溶液(含0.02 mmol/L EDTA-2Na,pH为3.8)和甲醇为流动相,梯度洗脱,进样体积为10μL,流量为1.0 mL/min,柱温为30℃,采用二极管阵列检测器,检测波长为230 nm。16种防腐剂的质量浓度在20~500 ng/mL范围内与色谱峰面积线性关系良好,相关系数均不小于0.9995,检出限为1~20 ng/mL,样品平均加标回收率为98.8%~102.5%,测定结果的相对标准偏差为0.78%~2.36%(n=9)。该方法操作简单,分离效果好,可用于阿胶糕中多种防腐剂的同时测定。
A high performance liquid chromatography method was established for simultaneous determination of 16 preservatives in Donkey-hide Gelatin Pastry,including benzoic acid,sorbic acid,dehydroacetic acid,salicylic acid,phenoxyisopropyl alcohol,2,6-dichlorobenzyl alcohol,methyl benzoate,iodopropyl alcohol butylcarbamate,p-chlormcresol,2,4 dichlorobenzyl alcohol,σ-cymene-5-ol,chlorocresol,clomibazol,benzyl chloride,triclocarban and sodium thiomersal.After extraction and protein removal,the Donkey-hide Gelatin Pastry was separated on a Kromasil C_(18) column(250 mm×4.6 mm,5μm)with 0.025 mol/L sodium dihydrogen phosphate solution(containing 0.02 mmol/L EDTA-2Na,pH 3.8)and methanol as the mobile phases,gradient elution.The injection volume was 10μL,the flow rate was 1.0 mL/min,the column temperature was 30℃,and the detection wavelength was 230 nm with a diode array detector.The mass concentration of 16 preservatives had a good linear relationship with the chromatographic peak area in the range of 20–500 ng/mL,the linear correlation coefficients were all not less than 0.9995,the detection limits were 1–20 ng/mL,the average recoveries of spiked samples were 98.8%–102.5%,and the relative standard deviations of the determination results were 0.78%–2.36%(n=9).The method has the advantages of simple operation and good separation,which can be used for the simultaneous determination of preservatives in Donkey-hide Gelatin Pastry.
作者
赵艳霞
张栋
姜岩
郭莹
周维利
高天阳
谢强胜
ZHAO Yanxia;ZHANG Dong;JIANG Yan;GUO Ying;ZHOU Weili;GAO Tianyang;XIE Qiangsheng(Shandong Institute for Food and Drug Control,National Medical Products Administration Key Laboratory for Quality Evaluation of Gelatin Products,Jinan 250101,China;Center for Food Evaluation,State Administration for Market Regulation,Beijing 100070,China)
出处
《化学分析计量》
CAS
2022年第6期63-67,共5页
Chemical Analysis And Meterage
关键词
阿胶糕
高效液相色谱法
防腐剂
Donkey-hide Gelatin Pastry
high performance liquid chromatography
preservatives
