安全监测

血液透析器中4,4’-二氨基二苯甲烷溶出量的测定及其允许限量的建立

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  • 1.苏州苏大卫生与环境技术研究所有限公司,苏州 215123;
    2.苏州大学苏州医学院,苏州 215123
第一作者 Tel:13716186034;E-mail:kingsunny1222@sina.com

修回日期: 2022-06-10

  网络出版日期: 2024-06-24

Determination of 4,4’-diaminodiphenyl methane released in hemodialyzer and establishment of allowable limits

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  • 1. Sanitation & Environment Technology Institute, Soochow University Ltd, Suzhou 215123, China;
    2. Suzhou Medical College, Soochow University, Suzhou 215123, China

Revised date: 2022-06-10

  Online published: 2024-06-24

摘要

目的: 采用极限浸提法提取血液透析器中的4,4’-二氨基二苯甲烷(MDA),建立HPLC测定血液透析器中MDA溶出量的方法并确立其允许限量。方法: 分别用甲醇-水(1∶1)和甲醇提取血液透析器中的MDA,采用Sun Fire C18(4.6 mm×250 mm,5 μm)色谱柱,光电二极管阵列(PDA)检测器全扫确定最优检测波长;进样量为10 μL;流动相:甲醇-磷酸盐缓冲液(25∶75),经22 min梯度洗脱至甲醇-磷酸盐缓冲液(55∶45),23 min变为去离子水(100)运行至28 min,29 min变为甲醇-磷酸盐缓冲液(25∶75)运行至37 min;流速为1.0 mL·min-1;柱温为40 ℃。结果: 甲醇-水(1∶1)浸提,PDA最优检测波长为242 nm,MDA质量浓度在0~2.03 μg·mL-1范围内线性关系良好(r2=0.999 8),定量限为0.081 μg·mL-1,仪器精密度和回收率优,测定MDA溶出量为59.7 μg;甲醇浸提,PDA最优检测波长为240 nm,MDA质量浓度在0~2.04 μg·mL-1范围内线性关系良好(r2=0.999 7),定量限为0.067 μg·mL-1,仪器精密度优,但回收率相对较低,测定MDA溶出量为64.1 μg;血液透析器中MDA溶出的允许限量为0.105 mg·d-1结论: 本方法经方法学验证,可用于血液透析器中MDA溶出量的检测,但甲醇-水(1∶1)不能满足低浓度MDA极限浸提的要求,甲醇浸提液可经氮吹浓缩,实现极限浸提。

本文引用格式

孙金陆, 方菁嶷, 王玲玲, 汪莹莹, 李峰, 章晶晶 . 血液透析器中4,4’-二氨基二苯甲烷溶出量的测定及其允许限量的建立[J]. 药物分析杂志, 2022 , 42(9) : 1618 -1624 . DOI: 10.16155/j.0254-1793.2022.09.15

Abstract

Objective: To extract 4,4’-diaminodiphenyl methane (MDA) in hemodialyzer by exhaustive extraction, and to establish an HPLC method for determination of MDA releaseand its allowable limits (AL). Methods: MDA was extracted from hemodialyzer using methanol-water(1∶1) and methanol respectively. The Sun Fire C18(4.6 mm×250 mm, 5 μm) column was used to determine the optimal detection wavelength with a photo-diode array (PDA) detector. Injection volume was 10 μL and the mobile phase was methanol, phosphate buffer and deionized water. Gradient elution at the flow rate of 1.0 mL·min-1was applied. Column temperature was 40 ℃. Results: For methanol-water(1∶1), the optimal detection wavelength was 242 nm, the calibration curves of MDA had a good linear relationship (r2=0.999 8) in the concentration range of 0-2.03 μg·mL-1. The limit of quantification was 0.081 μg·mL-1, instrument precision and recovery rate were excellent and the result of MDA release was 59.7 μg. For methanol, the optimal detection wavelength was 240 nm, the calibration curves of MDA had a good linear relationship (r2=0.999 7) in the concentration range of 0-2.04 μg·mL-1, the limit of quantification was 0.067 μg·mL-1,the instrument precision was good, but the recovery rate was relatively low.The result of MDA release was 64.1 μg. The AL of MDA release in hemodialyzer was 0.105 mg·d-1. Conclusion: This method is validated for determination of MDA release in hemodialyzer, but methanol-water (1∶1) is not suitable for the exhaustive extraction with low MDA concentration. Methanol extract can be concentrated by nitrogen blowing to complete the exhaustive extraction.

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