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《化学分析计量》 2022年第06期
DOI:10.3969/j.issn.1008-6145.2022.06.015
高效液相色谱法同时测定阿胶糕中16种防腐剂
赵艳霞1,张栋1,姜岩2,郭莹1,周维利1,高天阳1,谢强胜1
1.山东省食品药品检验研究院,国家药品监督管理局胶类产品质量评价重点实验室,济南 250101; 2.国家市场监督管理总局食品审评中心,北京 100070 
Simultaneous determination of 16 preservatives in Donkey-hide Gelatin Pastry by high performance liquid chromatography
ZHAO Yanxia1, ZHANG Dong1, JIANG Yan2, GUO Ying1, ZHOU Weili1, GAO Tianyang1, XIE Qiangsheng1
1. Shandong Institute for Food and Drug Control, National Medical Products AdministrationKey Laboratory for Quality Evaluation of Gelatin Products, Jinan 250101, China; 2. Center for Food Evaluation, State Administration for Market Regulation, Beijing 100070, China 
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色谱柱(250 18 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0.999 5,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。 
Abstract: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-chlorm- cresol, 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 column 18 (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 0.999 5, 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. 
关键词:阿胶糕;高效液相色谱法;防腐剂 
Keywords:Donkey-hide Gelatin Pastry; high performance liquid chromatography; preservatives 
本文引用格式:
赵艳霞,张栋,姜岩,等.高效液相色谱法同时测定阿胶糕中16种防腐剂[J].化学分析计量,2022,31(6):63.
ZHAO Yanxia,ZHANG Dong,JIANG Yan,et al. Simultaneous determination of 16 preservatives in Donkey-hide Gelatin Pastry by high performance liquid chromatography[J]. Chemical Analysis and Meterage,2022,31(6):63. 

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