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目的:建立同时测定复方磷酸可待因口服溶液中3种有效成分(磷酸可待因、盐酸麻黄碱、马来酸氯苯那敏)及2种防腐剂(苯甲酸钠、羟苯乙酯)含量的方法。 方法:采用高效液相色谱法。色谱柱为GL·Science WondaSil C18-WR,流动相为乙腈-0.01 mol/L磷酸二氢钾溶液(含2.5 mmol/L庚烷磺酸钠和0.1%三乙胺,用磷酸调节pH至2.5±0.1)(梯度洗脱),流速为1.0 mL/min,检测波长为210 nm,柱温为30 ℃,进样量为10 μL。 结果:磷酸可待因、盐酸麻黄碱、马来酸氯苯那敏、苯甲酸钠、羟苯乙酯检测质量浓度线性范围分别为0.365 8~457.20 μg/mL(r=0.999 9)、0.363 5~454.35 μg/mL(r=0.999 9)、0.124 8~155.98 μg/mL(r=0.999 9)、0.390 6~488.25 μg/mL(r=0.999 9)、0.121 3~151.65 μg/mL(r=0.999 9);定量限分别为0.409 4、0.508 8、7.731 4、1.347 6、1.940 8 ng,检测限分别为0.146 2、0.181 7、2.494 0、0.449 2、0.606 5 ng;精密度、稳定性、重复性试验的RSD均小于1%;加样回收率分别为98.10%~101.96%(RSD=1.4%,n=9)、97.65%~101.14%(RSD=1.2%,n=9)、97.30%~102.30%(RSD=1.8%,n=9)、97.71%~102.21%(RSD=1.5%,n=9)、97.03%~101.55%(RSD=1.7%,n=9)。 结论:该方法操作简单,精密度、稳定性、重复性均较好,可用于同时测定复方磷酸可待因口服溶液中磷酸可待因、盐酸麻黄碱、马来酸氯苯那敏、苯甲酸钠和羟苯乙酯的含量。
OBJECTIVE: To establish a method for simultaneous determination of 3 active components as codeine phosphate, ephedrine hydrochloride, chlorphenamine maleate and 2 preservatives as sodium benzoate and ethylparaben in Compound codeine phosphate oral solution. METHODS: HPLC method was adopted. The determination was performed on GL·Science WondaSil C18-WR column with mobile phase consisted of acetonitrile-0.01 mol/L potassium dihydrogen phosphate solution (containing 2.5 mmol/L sodium heptane sulfonate and 0.1% triethylamine, pH adjusted to 2.5±0.1 with phosphoric acid) (gradient elution) at the flow rate of 1.0 mL/min. The detection wavelength was set at 210 nm and column temperature was 30 ℃. The sample size was 10 μL. RESULTS: The linear ranges of codeine phosphate, ephedrine hydrochloride, chlorphenamine maleate, sodium benzoate and ethylparaben were 0.365 8-457.20 μg/mL (r=0.999 9), 0.363 5-454.35 μg/mL (r=0.999 9), 0.124 8-155.98 μg/mL (r=0.999 9), 0.390 6-488.25 μg/mL (r=0.999 9), 0.121 3-151.65 μg/mL(r=0.999 9), respectively. The limits of quantitation were 0.409 4, 0.508 8, 7.731 4, 1.347 6, 1.940 8 ng; the limits of detection were 0.146 2, 0.181 7, 2.494 0, 0.449 2, 0.606 5 ng. RSDs of precision, stability and reproducibility tests were all lower than 1%. The average recoveries were 98.10%-101.96%(RSD=1.4%,n=9), 97.65%-101.14%(RSD=1.2%,n=9), 97.30%-102.30% (RSD=1.8%,n=9), 97.71%-102.21%(RSD=1.5%,n=9), 97.03%-101.55%(RSD=1.7%,n=9), respectively. CONCLUSIONS: The method is simple, precise, stable and reproducible, and it can be used for simultaneous determination of codeine phosphate, ephedrine hydrochloride, chlorphenamine maleate, sodium benzoate and ethylparaben in Compound codeine phosphate oral solution.
复方磷酸可待因口服溶液高效液相色谱法磷酸可待因盐酸麻黄碱马来酸氯苯那敏苯甲酸钠羟苯乙酯含量测定
Compound codeine phosphate oral solutionHPLCCodeine phosphateEphedrine hydrochlorideChlorphenamine maleateSodium benzoateEthylparabenContent determination
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