HPLC法测定赖氨酸维B12颗粒中香草醛的含量

Determination of vanillin in lysine and vitamin B12 granules by HPLC

田海燕 ¹刘娟 ¹刘维彬 ¹刘洪海¹

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作者信息

1. 德州市食品药品检验检测中心,山东德州 253000
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摘要

目的:建立HPLC法测定赖氨酸维B12颗粒中香草醛含量的方法.方法:取赖氨酸维B12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Agi-lent C18(250 mm ×4.6 mm,5 μm)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0.2 μg·g-1,浓度在1.962～49.04μg·mL-1的范围内呈线性关系(r=0.999 9),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B12颗粒中香草醛含量的测定.

Abstract

Objective:To establish an HPLC method to determine of vanillin in lysine and vitamin B12 granules.Methods:1.0 g of lysine and vitamin B12 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 1 min for extraction.The samples were separated on a C18 column(250 mm × 4.6 mm,5 μm)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 0.2 µg·g-1,and the concentration was linear in the range of 1.962-49.04 µg·mL-1(r=0.999 9).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 55.18-79.55 μg·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 B12 granules.

关键词

赖氨酸维B12颗粒/香草醛/含量/HPLC法/辅料/矫味剂

Key words

lysine and vitamin B12 granules/vanillin/HPLC method/pharmaceutical excipient/flavoring agent

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出版年

2024

中国药品标准

国家药典委员会

中国药品标准

影响因子：0.372

ISSN：1009-3656

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