高效液相色谱法同时检测某水溶性聚合物中三种单体含量

Simultaneous Determination of Three Residual Monomers in Water-soluble Polymer by HPLC

刘华沙 李菁菁 刘思伽 孙 强

LIU Huasha LI Jingjing LIU Sijia SUN Qiang

针对水溶性聚合物残余单体的检测方法针对性太强的问题，建立了一种同时测定某水溶性聚合物中三种单体（顺式丁烯二酸、反式丁烯二酸和衣康酸）质量分数的高效液相色谱（HPLC）分析方法。实验条件经优化后确定为：前处理过程为采用乙腈对该水溶性聚合物进行萃取 30 min，再以0.1%磷酸水溶液-乙腈（85∶15）进行等度洗脱，使用安捷伦Zorbax Eclipse XDB C18色谱柱（250×4.6 mm，5 μm），柱流速为0.8 mL/min，柱温为45 ℃，检测波长为 210 nm。实验发现：该水溶性聚合物中3种残余单体分离度良好（分离度大于3），线性关系良好（R2大于 0.999），稳定性良好（RSD 小于 1%）；顺式丁烯二酸、反式丁烯二酸和衣康酸的最小检测限分别为 0.32、0.34、 0.63 mg/kg；顺式丁烯二酸、反式丁烯二酸和衣康酸的最小限定限分别为1.21、1.26 、2.02 mg/kg；3种单体的加标回收率均在 98%～101%之间。某钻井液用增黏剂样品中上述 3 种单体的质量分数的依次为 2.261%、0.284%、 2.775%。该方法可以准确控制水溶性聚合物的合成过程，实现对其进行精准质量控制。色谱检测时间小于10 min，高效准确，可实现对该水溶性聚合物的质量控制。

As for the problem that the detection method of residual monomer of water-soluble polymer was too targeted，a method for simultaneous determination of maleic acid，fumaric acid and itaconic acid in water-soluble polymer used in drilling fluid by HPLC was established. The experimental conditions were obtained as follows：the water-soluble polymer was extracted with acetonitrile for 30 min，and the mobile phase contained 0.1% phosphoric acid and acetonitrile at volume ratio 85∶15. Agilent Zorbax Eclipse XDB C18 column（250 × 4.6 mm，5 μm）was used，and the flow rate of column was 0.8 mL/min，the column temperature was 45 ℃，and the detection wavelength was 210 nm. Under the above experimental conditions，the detection results had good separation characteristics（the separation degree was greater than 3），good linear relationship（the R2 value was greater than 0.999）and good stability（the RSD was less than 1%）. The minimum detection limit of maleic acid，fumaric acid and itaconic acid were 0.32，0.34 and 0.63 mg/kg. the quantitation of maleic acid，fumaric acid and itaconic acid were 1.21，1.26 and 2.02 mg/kg. The recoveries of the three residual monomers were 98%—101%. The mass fractions of the three residual monomers in a sample of the viscosifier were 2.261%，0.284% and 2.775%. The time of chromatographic detection was less than 10 min，and it could meet the quality control of the water-soluble polymer. The method could accurately control the synthesis process of water-soluble polymers and achieve accurate quality control.

10.19346/j.cnki.1000-4092.2025.01.021