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作 者:田海燕 刘娟 刘维彬 刘洪海 TIAN Haiyan;LIU Juan;LIU Weibin;LIU Honghai(Dezhou Institute for Food and Drug Control,Dezhou 253000,China)
机构地区:[1]德州市食品药品检验检测中心,山东德州253000
出 处:《中国药品标准》2024年第5期517-520,共4页Drug Standards of China
摘 要:目的:建立HPLC法测定赖氨酸维B_(12)颗粒中香草醛含量的方法。方法:取赖氨酸维B_(12)颗粒1.0 g,置10 mL刻度离心管中,加水1 mL溶解后,涡旋1 min,加甲醇至刻度后,继续涡旋1 min进行提取。采用Agilent C 18(250 mm×4.6 mm,5μm)色谱柱,流动相为甲醇-水(35:65),检测波长为277 nm。结果:本方法香草醛检出限为0.2μg·g^(-1),浓度在1.962~49.04μg·mL^(-1)的范围内呈线性关系(r=0.9999),低、中、高三水平回收率在91.86%~101.61%之间,RSD为2.9%(n=9)。测定样品6批,A企业4批,香草醛含量在55.18~79.55μg·g^(-1),B企业和C企业均未检出。结论:该方法操作简便,结果可靠,可用于赖氨酸维B 12颗粒中香草醛含量的测定。Objective:To establish an HPLC method to determine of vanillin in lysine and vitamin B_(12)granules.Methods:1.0 g of lysine and vitamin B_(12)granules was put into a 10mL graduated centrifuge tube,1 mL of water was added to dissolve,vortex for 1 min,and methanol was added to the scale and vortex for 1min for extraction.The samples were separated on a C_(18)column(250 mm×4.6 mm,5μm)with a mobile phase of methanol and water(35∶65)at ta flow rate of 1.0 mL·min^(-1).The detection wavelength was 277 nm.Results:The limit of detection of vanillin was 0.2μg·g^(-1),and the concentration was linear in the range of 1.962-49.04μg·mL^(-1)(r=0.9999).The recoveries of vanillin at low,medium and high levels were 91.86%-101.61%with RSD of 2.9%(n=9).6 batches of samples were determined,and the results showed that the vanillin content in 4 batches of enterprise A was 55.18-79.55μg·g^(-1),and no vanillin was detected in enterprise B and enterprise C.Conclusion:The method is simple and reliable,and can be used for the rapid determination of vanillin in lysine and vitamin B_(12)granules.
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