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超高效液相色谱-串联质谱法测定牙膏中36种抗感染类药物

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建立了超高效液相色谱-串联质谱法同时测定牙膏中36种抗感染类药物的检测方法.样品先采用饱和氯化钠溶液分散后用乙腈超声提取,经色谱柱Phenomenex Kinetex C18(50×3.0 mm,2.6 pm)分离,以乙酸铵溶液和乙腈溶液梯度洗脱,采用电喷雾离子源正负离子模式电离,多反应监测(MRM)模式检测.结果表明,36种抗感染类药物在50~800 ng/mL范围内线性关系良好,相关系数均大于0.99;检出限为0.003~0.250 μg/g,平均回收率为78.1%~119.2%,相对偏差RSD为0.6%~8.5%.应用该方法对20批市售牙膏样品进行测定,均未检出该类抗感染类药物.该方法具有良好的灵敏度、精密度及准确度,能够用于牙膏中抗感染类药物的测定.
Determination of 36 anti-infective drugs in toothpaste by UPLC
A highly efficient liquid chromatography-tandem mass spectrometry(LC-MS/MS)method was established for the simultaneous determination of 36 anti-infective drugs in toothpaste.Samples were first dispersed with saturated sodium chlo-ride solution and then extracted with acetonitrile using ultrasonication.Separation was achieved through the Phenomenex Kinetex C18 chromatographic column(50×3.0 mm,2.6 pm),with gradient elution using ammonium acetate solution and ace-tonitrile.Ionization was performed in both positive and negative ion modes using an electrospray ionization(ESI)source,and the compounds were detected using multiple reaction monitoring(MRM)mode.The results demonstrated that the 36 an-ti-infective drugs had good linear relationships within the range of 50-800 ng/mL,with correlation coeffiicients greater than 0.99.The limits of detection(LOD)ranged from 0.003 to 0.250 µg/g,with average recoveries between 78.1%-119.2%,and rel-ative standard deviations(RSD)ranging from 0.6%-8.5%.When the method was applied to test 20 batches of commercially available toothpaste samples,none of these anti-infective drugs were detected.The method exhibits good sensitivity,precision and accuracy,making it suitable for the determination of anti-infective drugs in toothpaste.

UPLCToothpasteAnti-infective drugs

邓丽华、刘颖强、陈洪骏

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肇庆市药品检验所 广东肇庆 526000

超高效液相色谱-串联质谱法 牙膏 抗感染类药物

2024

质量安全与检验检测
中国检验检疫科学研究院

质量安全与检验检测

影响因子:0.399
ISSN:2096-8876
年,卷(期):2024.34(6)