Determination of docusate sodium by ion-pair high-performance liquid chromatography
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摘要:
为降低对高载碳量色谱柱的依赖，优化并建立了多库酯钠含量测定的新型离子对高效液相色谱法（IP-HPLC）。采用四丙基氯化铵为离子对试剂，乙腈-10 mmol/L四丙基氯化铵水溶液（66∶34）为流动相，用0.1%磷酸溶液调pH至6.5，流速为1.5 mL/min，检测波长为214 nm，柱温为35 ℃，进样量为25 μL，外标法测定。结果表明该方法专属性良好，主峰拖尾因子为1.34；在0.02~0.40 mg/mL范围内线性关系良好，相关系数r=
0.9999 ；重复性结果良好，加样回收率97.0%~98.2%（n=6）；定量限为3.31 μg/mL；检测限为2.76 μg/mL。总体来看，新方法耐用性好、线性范围宽、灵敏度高，适合用于测定多库酯钠的含量。Abstract:To reduce the dependency on high-carbon-load chromatographic columns,a new method has been established for the determination of the content of docusate sodium using ion-pair high-performance liquid chromatography (IP-HPLC). Tetrapropylammonium chloride was used as the ion-pair reagent with a mobile phase, composition of acetonitrile:10 mmol/L tetrapropylammonium chloride solution = 66∶34, adjusting pH to 6.5 with 0.1% phosphoric acid solution,flow rate of 1.5 mL/min, detection wavelength of 214 nm,column temperature of 35 °C, and an injection volume of 25 μL,and quantified by an external standard method. The main peak of docusate sodium exhibited a tailing factor of 1.34. The method showed good linearity within the range of 0.02 mg/mL to 0.40 mg/mL, with a correlation coefficient (r) of 0.999 9. It also demonstrated good repeatability, with recovery ranging from 97.0% to 98.2% (n=6). The quantification limit was 3.31 μg/mL, and the detection limit was 2.76 μg/mL.In summary,the new method shows good durability, a wide linear range, and high sensitivity, it is suitable for the determination of docusate sodium.
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Figure 1. Chromatograms and retention behavior at different pH conditions
A：pH 7.51; B：pH 6.48;C：pH 5.51;D：pH 4.50;E：pH 3.61
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Figure 3. Chromatographic performance results of the USP method in different loading columns(DS:Docusate sodium)
A:Thermo Hypersil GOLD;B:GL Sciences ODS-3;C:Waters Symmetry C18;D:Phenomenex Ultracarb ODS(30)60 Å
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Figure 4. Chromatographic performance results of the new method in different loading columns
A:Thermo Hypersil GOLD; B:GLSciences ODS-3;C:Waters Symmetry C18;D:Phenomenex UltracarbODS(30)60 Å
Table 1 Effect of ions pair type on the separation performance
Ion pair type tR/min Peak area Plate number Symmetry factor Tetramethylammonium chloride 3.03 50050 643 1.49 Tetraethylammonium chloride 4.65 45173 454 1.14 Tetrapropylammonium chloride 5.21 47084 1637 1.50 Tributylmethylammonium chloride 6.50 48425 2112 1.47 Tetrabutylammonium chloride 7.40 57387 1585 1.18 Tetrapentylammonium chloride 14.15 31807 2705 1.27 
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Table 2 Results of forced degradation testing
Conditions Peak area ratio/% Main peak Impurity A Impurity B Impurity C Impurity D Others Untreated 98.08 1.76 / 0.16 / / High temperature 98.29 1.53 / 0.18 / / Light exposure 97.36 2.49 / 0.15 / / Strong acid 97.08 2.92 / / / / Strong alkali 86.01 13.99 / / / / Oxidation 96.16 3.84 / / / / /:Not detected
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Table 3 HPLC results and titration results for samples from three manufacturers
Manufacturer Batch No. New method ChP2020(1st Suppl.) method Main component Total impurity Domestic Company A 211106 96.8% 0.5% 97.2% Domestic Company B T202111YC02 92.7% 0.9% 94.8% Import Company A WS21F0803 95.6% 3.7% 97.5%
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Table 4 Column type specifications
No. Brand Type Carbon loading/% A Thermo Hypersil GOLD, 250 mm×4.6 mm,5 μm 10 B GL Sciences ODS-3, 250 mm×4.6 mm,5 μm 15 C Waters Symmetry C18, 250 mm×4.6 mm,5 μm 20 D Phenomenex Ultracarb,150 mm×4.6 mm,5 μm 30
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