首页|UPLC-PDA测定鲜竹沥中4种抑菌剂的含量

UPLC-PDA测定鲜竹沥中4种抑菌剂的含量

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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.
Determination of Four Preservatives in Fresh Bamboo Juice by UPLC-PDA Method
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.

bamboo juicepreservativesUPLCcontent determination

张贤睿、王莹、金红宇、魏锋、马双成

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中国药科大学,江苏 南京 211198

中国食品药品检定研究院,北京 102629

国家药典委员会,北京 100061

鲜竹沥 抑菌剂 超高效液相色谱法 含量测定

2024

中国现代中药
中国中药协会,中国医药集团总公司,中国药材公司

中国现代中药

CSTPCD
影响因子:0.65
ISSN:1673-4890
年,卷(期):2024.26(5)
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