| 摘要: |
| 目标：建立离子色谱-抑制电导检测法测定化学对照品中酒石酸盐的含量。方法：以酒石酸沃尼妙林对照品为例,采用DIONEX IonPac AS19(250 mm×4 mm)阴离子交换色谱柱和Ion Pac AS19保护柱(50 mm×4.0 mm),以22 mmol.L-1氢氧化钾溶液为流动相,流速为1.0 mL.min-1等度洗脱,抑制电导检测器检测,测定酒石酸盐中酒石酸的含量。结果：该方法在1.0~50 μg.mL-1浓度范围内线性关系良好(r=0.999),定量限为0.5μg.mL-1,酒石酸沃尼妙林在3个水平的加样回收率分别为98.79%、98.91%与96.50%,平均回收率为98.07% (RSD=2.20%,n=9)。用此方法测定3个厂家共5批样品,酒石酸沃尼妙林中酒石酸含量的数值与理论值基本一致。结论：本文建立的离子色谱法准确、灵敏,可用于酒石酸盐成盐比例与含量的测定。 |
| 关键词: 离子色谱法 化学对照品 酒石酸 酒石酸沃尼妙林 |
| DOI： |
| 投稿时间：2023-11-28修订日期：2024-03-05 |
| 基金项目:中国兽医药品监察所“兽药行业公益性重点专项”( No: GY202107) |
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| Determination of Tartaric Acid in Valnemulin Tartrate by Ion Chromatography |
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| (Safety Assessment Department,China Institute of Veterinary Drug Control,Beijing,100081;China) |
| Abstract: |
| ABSTRACT: OBJECTIVE To establish an ion chromatography method with suppressed conductivity detection for the tartaric acid salt determination in the chemical reference standards. METHODS The tartaric acid salt content of valnemulin tartrate was determined by an Ion Pac AS19 anion exchange column (250mm×4.0mm) and Ion Pac AS19 guard column(50 mm×4.0 mm), using suppressed conductivity detector. An isocratic eluent of 22 mmol·L-1 KOH was chosen as mobile phase, flow rate was 1.0 mL·min-1. RESULTS A good linear relationship was observed within the range of 1.0~50.0 μg·mL-1 (r=0.999, n=6). The limit of quantification was 0.5 μg·mL-1. The average spiked recovery was 98.07% at three concentration levels with RSD of 2.20% (n=9). Five batches of samples from 3 manufactures were tested using this validated method, and no significant difference was found between the samples, the salt-forming rate of valnemulin and tartaric acid in the samples of valnemulin tartrate is reasonable and qualified. CONCLUSION The method is accurate，sensitive and simple，which provides a reliable analytical method for the control of tartaric acid salt content in the chemical reference standards. |
| Key words: ion chromatography chemical reference standards tartaric acid valnemulin tartrate |
