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反相高效液相色谱法同时测定五味香连丸中10种成分含量

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目的 建立同时测定五味香连丸中盐酸小檗碱、黄连碱、巴马汀、延胡索乙素、木香烃内酯、去氢木香内酯、吴茱萸碱、吴茱萸次碱、柠檬苦素、芍药苷 10 种成分含量的反相高效液相色谱法。方法 色谱柱为Waters SunFire C18 柱(250 mm×4。6 mm,5 μm),流动相为含 0。02%三乙胺的 0。02 mol/L磷酸二氢钾溶液(用磷酸调pH至 3。5)-乙腈(梯度洗脱),流速为 1。0 mL/min,柱温为 35℃,检测波长为 225 nm,进样量为 10 μL。结果 盐酸小檗碱、黄连碱、巴马汀、延胡索乙素、木香烃内酯、去氢木香内酯、吴茱萸碱、吴茱萸次碱、柠檬苦素、芍药苷的质量浓度分别在 6。852~51。39 μg/mL、2。956~22。17 μg/mL、2。918~21。88 μg/mL、4。643~34。82 μg/mL、4。871~36。53 μg/mL、4。007~30。05 μg/mL、4。519~33。89 μg/mL、4。482~33。62 μg/mL、2。724~20。43 μg/mL、2。809~21。07 μg/mL范围内与峰面积线性关系良好(r≥0。999 2,n = 6);定量限分别为 0。66,0。31,0。29,0。45,0。48,0。41,0。42,0。46,0。27,0。28 μg/mL;精密度、稳定性、重复性试验结果的RSD均小于 2。0%(n = 6);回收率分别为100。36%,98。74%,98。71%,99。67%,99。86%,99。59%,98。70%,98。38%,98。25%,98。72%,RSD 分别为0。89%,1。02%,1。04%,1。17%,0。84%,1。15%,1。33%,1。20%,1。07%,1。23%(n = 6)。3 批样品中上述成分的平均含量分别为 1。165~1。192 mg/g、0。523 1~0。527 6 mg/g、0。499 7~0。501 1 mg/g、0。681 4~0。688 9 mg/g、0。697 7~0。700 2 mg/g、0。606 8~0。613 4 mg/g、0。580 1~0。583 7 mg/g、0。427 7~0。442 2 mg/g、0。410 1~0。416 5 mg/g、0。400 2~0。401 3 mg/g(n = 2)。结论 所建立的方法简便可行、结果准确可靠、稳定性好,可用于同时测定五味香连丸中 10 种成分的含量。
Simultaneous Determination of 10 Components in Wuwei Xianglian Pills by RP-HPLC
Objective To establish a reverse-phase high-performance liquid chromatography(RP-HPLC)method for the simultaneous determination of 10 components in Wuwei Xianglian Pills,including berberine ydrochloride,coptisine,palmatine,tetrahydropalmatine,costunolide,dehydrocostuslactone,evodiamine,rutaecarpine,limonin,and paeoniflorin.Methods The chromatography column was Waters SunFire C18 column(250 mm×4 6 mm,5 μm),the mobile phase was 0.02 mol/L potassium dihydrogen phosphate solution containing 0.02%triethylamine(the pH was ajusted to 3.5 with phophoric acid)-acetonitrile(gradient elution),the flow rate was 1.0 mL/min,the column temperature was 35℃,the detection wavelength was 225 nm,and the injection volume was 10 μL.Results The linear ranges of berberine hydrochloride,coptisine,palmatine,tetrahydropalmatine,costunolide,dehydrocostuslactone,evodiamine,rutaecarpine,limonin and paeoniflorin were 6.852-51.39 μg/mL,2.956-22.17 μg/mL,2.918-21.88 μg/mL,4.643-34.82 μg/mL,4.871-36.53 μg/mL,4.007-30.05 μg/mL,4.519-33.89 μg/mL,4.482-33.62 μg/mL,2.724-20.43 μg/mL,and 2.809-21.07 μg/mL(r≥0.999 2,n = 6),respectively.The limits of quantification(LOQ)were 0.66,0.31,0.29,0.45,0.48,0.41,0.42,0.46,0.27,0.28 μg/mL,respectively.The RSDs of precision,stability,and repeatability test results were all lower than 2.0%(n = 6).The average recoveries of the above 10 components were 100.36%,98.74%,98.71%,99.67%,99.86%,99.59%,98.70%,98.38%,98.25%,98.72%,with RSDs of 0.89%,1.02%,1.04%,1.17%,0.84%,1.15%,1.33%,1.20%,1.07%,and 1.23%(n = 6),respectively.The average contents of the above 10 components in three batches of samples were 1.165-1.192 mg/g,0.523 1-0.527 6 mg/g,0.499 7-0.501 1 mg/g,0.681 4-0.688 9 mg/g,0.697 7-0.700 2 mg/g,0.606 8-0.613 4 mg/g,0.580 1-0.583 7 mg/g,0.427 7-0.442 2 mg/g,0.410 1-0.416 5 mg/g,and 0.400 2-0.401 3 mg/g(n = 2),respectively.Conclusion The established method is convenient and feasible,with accurate and reliable results and good stability,which can be used for the simultaneous determination of 10 components in Wuwei Xianglian Pills.

RP-HPLCWuwei Xianglian Pillscontent determination of multi-components

吴璐叶、杨正英、于上林

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中国人民解放军联勤保障部队第九○○医院,福建 福州 350000

反相高效液相色谱法 五味香连丸 多成分含量测定

2024

中国药业
重庆市食品药品监督管理局

中国药业

CSTPCD
影响因子:1.369
ISSN:1006-4931
年,卷(期):2024.33(9)
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