UPLC-PDA测定鲜竹沥中4种抑菌剂的含量
投稿时间:2024-01-02     点此下载全文
引用本文:张贤睿,王莹,金红宇,魏锋,马双成.UPLC-PDA测定鲜竹沥中4种抑菌剂的含量[J].中国现代中药,2024,26(5):869-873
DOI:10.13313/j.issn.1673-4890.20240102004
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作者中文名作者英文名单位中文名单位英文名E-Mail
张贤睿 ZHANG Xian-rui 中国药科大学,江苏 南京 211198 China Pharmaceutical University, Nanjing 211198, China  
王莹* WANG Ying 中国食品药品检定研究院,北京 102629 National Institutes for Food and Drug Control, Beijing 102629, China  
金红宇 JIN Hong-yu 中国食品药品检定研究院,北京 102629 National Institutes for Food and Drug Control, Beijing 102629, China  
魏锋 WEI Feng 中国食品药品检定研究院,北京 102629 National Institutes for Food and Drug Control, Beijing 102629, China  
马双成 MA Shuang-cheng 国家药典委员会,北京 100061 Chinese Pharmacopoeia Commission, Beijing 100061, China  
中文摘要:目的 建立超高效液相色谱-二极管阵列检测器法(UPLC-PDA)检测市售鲜竹沥中苯甲酸、山梨酸、羟苯甲酯、羟苯乙酯4种常用抑菌剂的含量。方法 采用ACQUITY UPLC HSS T3色谱柱(100 mm×2.1 mm,1.8 μm),以乙腈(A)-0.02mol·L–1乙酸铵溶液(B)为流动相梯度洗脱,流速0.3 mL·min–1,采用223 nm(苯甲酸)、254 nm(山梨酸、羟苯甲酯、羟苯乙酯)作为检测波长,进样量1 μL,柱温30 ℃。结果 4种抑菌剂在其测定波长下均完全分离,4种抑菌剂平均加样回收率分别为97.9%、104.0%、99.2%、103.0%;重复性试验苯甲酸和羟苯乙酯峰面积的RSD(n=6)均小于1%;4种抑菌剂质量浓度与峰面积均呈良好线性关系(r均大于0.999 45);且样品的稳定性较好,48 h内苯甲酸峰面积的RSD为1.47%,羟苯乙酯峰面积的RSD为0.2%,对13批鲜竹沥中的抑菌剂进行了检测,9批鲜竹沥检出苯甲酸(质量分数为0.07%~0.29%),2批鲜竹沥检出山梨酸(质量分数为0.21%~0.24%),2批鲜竹沥检出苯甲酸(质量分数为0.21%~0.22%)和羟苯乙酯(质量分数为0.025%~0.027%),均符合《中华人民共和国药典》2020版(四部)通则0181合剂项下要求。结论 建立了基于UPLC-PDA测定鲜竹沥中的4种常用抑菌剂含量的方法,该方法专属性、重复性、准确度良好,为鲜竹沥这一冷背品种的质量控制提供了参考。
中文关键词:鲜竹沥  抑菌剂  超高效液相色谱法  含量测定
 
Determination of Four Preservatives in Fresh Bamboo Juice by UPLC-PDA Method
Abstract:To establish a ultrahigh performance liquid chromatography-diode array detector (UPLC-PDA) method to detect the contents of four commonly used preservatives in commercially available fresh bamboo juice, including benzoic acid, sorbic acid, methylparaben, and ethylparaben.Methods The ACQUITY UPLC HSS T3 column (100 mm×2.1 mm, 1.8 μm) was used with a gradient elution of acetonitrile as mobile phase A and 0.02 mol·L–1 ammonium acetate as mobile phase B at a flow rate of 0.3 mL·min–1. The 223 nm (benzoic acid) and 254 nm (sorbic acid, methylparaben and ethylparaben) were used as detection wavelengths, the injection volume was 1 μL, and the column temperature was 30 ℃.Results The four preservatives were all completely separated at their determination wavelengths, and the average recoveries of the four preservatives were 97.9%, 104.0%, 99.2% and 103.0%, respectively; the RSDs (n=6) of the peak areas of benzoic acid and ethylparaben in the repeatability test were both <1%; the mass concentrations of the four preservatives showed a good linear relationship with the peak area (r all >0.999 45); and the samples had a good stability. The RSD of the peak area of benzoic acid within 48 h was 1.47%, and the RSD of the peak area of ethylparaben within 48 h was 0.2%. The preservatives in 13 batches of fresh bamboo juice were detected, benzoic acid was detected in 9 batches of fresh bamboo juice (mass fraction of 0.07%-0.29%), sorbic acid was detected in 2 batches of fresh bamboo juice (mass fraction of 0.21%- 0.24%), benzoic acid (mass fraction of 0.21%-0.22%) and ethylparaben (mass fraction of 0.025%-0.027%) were detected in 2 batches of fresh bamboo juice, all of which met the requirements in Section of Mixture of the General Rule 0181 in the Chinese Pharmacopoeia (2020 version) Volume Ⅳ.Conclusion A method for determining the contents of four commonly used preservatives in fresh bamboo juice is established based on UPLC-PDA, and the method has good specificity, reproducibility and accuracy, which provides a reference for the quality control of fresh bamboo juice, a product which is not used on a large scale.
keywords:bamboo juice  preservatives  UPLC  content determination
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