高效液相色谱法同时测定小儿四维葡钙片中6种成分含量OA
Content Determination of Six Components in Xiao'er Siwei Pugai Tablets by HPLC
目的 建立同时测定小儿四维葡钙片中 6 种成分含量的高效液相色谱法.方法 采用高效液相色谱法测定制剂中葡萄糖、蔗糖、维生素D2 的含量,采用超高效液相色谱法测定制剂中维生素B1、维生素B2、维生素C的含量.色谱柱,葡萄糖和蔗糖为Ultimate XB-NH2氨基柱(250 mm×4.6 mm,5 μm),维生素B1、维生素B2、维生素C为Acquity UPLC HSS T3柱(150 mm×2.1 mm,1.8 μm),维生素D2为广州研创Gensial®C18 柱(150 mm×4.6 mm,5 μm);流动相,葡萄糖和蔗糖为乙腈-水-氨水(80∶20∶0.1,V/V/V),维生素B1、维生素B2、维生素C为 0.02mol/L磷酸二氢铵溶液(含 0.05%庚烷磺酸钠,用磷酸调pH至 3.0)-甲醇(80∶20,V/V),维生素D2 为乙腈-0.5%甲酸溶液(95∶5,V/V);流速,葡萄糖、蔗糖、维生素D2 为 1.0 mL/min,维生素B1、维生素B2、维生素C为 0.2 mL/min;检测波长,维生素B1、维生素B2、维生素C为 267 nm,维生素D2为 264 nm;检测器,葡萄糖和蔗糖为示差折光检测器,维生素B1、维生素B2、维生素C为二极管阵列(PDA)检测器,维生素D2 为紫外-可见分光光度检测器;柱温,葡萄糖、蔗糖、维生素D2 为 40℃,维生素B1、维生素B2、维生素C为 35℃;进样量,葡萄糖、蔗糖、维生素D2 为 10 μL,维生素B1、维生素B2、维生素C为 1 μL.结果 葡萄糖、蔗糖、维生素B1、维生素B2、维生素C、维生素D2 的质量浓度分别在 1.00～20.00 mg/mL、1.00～20.00 mg/mL、0.80～24.00 μg/mL、0.40～12.00 μg/mL、10.00～300.00 μg/mL、0.10～10.00 μg/mL范围内与峰面积线性关系良好(R2≥0.999 1);检测限分别为1.00 μg、2.00 μg、0.02 ng、0.01 ng、0.025 ng、0.20 ng,定量限分别为 3.00 μg、6.00 μg、0.80 ng、0.40 ng、0.10 ng、0.50 ng;精密度、稳定性、重复性试验结果的RSD均小于 2.50%;平均加样回收率分别为 99.18%,99.47%,98.83%,98.54%,99.49%,98.80%,RSD分别为 1.61%,2.28%,1.82%,2.47%,2.33%,2.72%(n=6).3 批样品中每片分别含以上 6 种成分 148.702～153.218 mg、148.623～151.419 mg、0.198～0.203 mg、0.098～0.103 mg、2.488～2.512 mg、1.632～1.689 μg.结论 该方法操作简便、专属性强、重复性好、结果准确,可用于同时测定小儿四维葡钙片中主要成分的含量.
Objective To establish a high-performance liquid chromatography(HPLC)method for the simultaneous determination of six components in Xiao'er Siwei Pugai Tablets.Methods The contents of glucose,sucrose,and vitamin D2 in the preparation were determined by the HPLC method,while the contents of vitamin B1,vitamin B2,and vitamin C in the preparation were determined by the ultra-high-performance liquid chromatography(UPLC)method.Chromatographic columns:the Ultimate XB-NH2 amino column(250 mm×4.6 mm,5 μm)was used for glucose and sucrose,the Acquity UPLC HSS T3 column(150 mm×2.1 mm,1.8 μm)was used for vitamin B1,vitamin B2 and vitamin C,and the Guangzhou Yanchuang Gensial® C18 column(150 mm×4.6 mm,5 μm)was used for vitamin D2.Mobile phases:acetonitrile-water-ammonia solution(80∶20∶0.1,V/V/V)was set for glucose and sucrose,0.02 mol/L ammonium dihydrogen phosphate solution(containing 0.05%sodium heptane sulfonate,adjusted to pH 3.0 with phosphoric acid)-methanol(80∶20,V/V)was set for vitamin B1,vitamin B2,and vitamin C,and acetonitrile-0.5%formic acid solution(95∶5,V/V)was set for vitamin D2.Flow rates:1.0 mL/min was set for glucose,sucrose,and vitamin D2,and 0.2 mL/min was set for vitamin B1,vitamin B2,and vitamin C.Detection wavelengths:267 nm was set for vitamin B1,vitamin B2,and vitamin C,and 264 nm was set for vitamin D2.Detectors:the UV-visible spectrophotometric refractive index detector was used for determining glucose and sucrose,the photo-diode array(PDA)detector was used for determining vitamin B1,vitamin B2,and vitamin C,and the UV-visible spectrophotometric detector was used for determining vitamin D2.Column temperatures:40℃was set for glucose,sucrose,and vitamin D2,and 35℃was set for vitamin B1,vitamin B2,and vitamin C.Injection volumes:10 μL was set for glucose,sucrose,and vitamin D2,and 1 μL was set for vitamin B1,vitamin B2,and vitamin C.Results The linear ranges for glucose,sucrose,vitamin B1,vitamin B2,vitamin C,and vitamin D2 were 1.00-20.00 mg/mL,1.00-20.00 mg/mL,0.80-24.00 μg/mL,0.40-12.00 μg/mL,10.00-300.00 μg/mL,and 0.10-10.00 μg/mL(R²≥0.999 1),respectively.The limits of detection of the above six components were 1.00 μg,2.00 μg,0.02 ng,0.01 ng,0.025 ng,and 0.20 ng,and the limits of quantification of the above six components were 3.00 μg,6.00 μg,0.80 ng,0.40 ng,0.10 ng,and 0.50 ng,respectively.The RSDs of the precision,stability,and repeatability tests were all lower than 2.50%.The average recoveries of the above six components were 99.18%,99.47%,98.83%,98.54%,99.49%,and 98.80%,with RSDs of 1.61%,2.28%,1.82%,2.47%,2.33%,and 2.72%(n=6),respectively.In the three batches of samples,the six components in each tablet were in the ranges of 148.702-153.218 mg,148.623-151.419 mg,0.198-0.203 mg,0.098-0.103 mg,2.488-2.512 mg,and 1.632-1.689 μg,respectively.Conclusion The method is simple,specific,reproducible,and accurate,which can be used for simultaneous determination of six components in Xiao'er Siwei Pugai Tablets.
夏方亮;顾晶晶;王建强;曹洪杰;雷永艳
山东省滨州市检验检测中心·山东省滨州市化学药物研发与质量控制重点实验室,山东 滨州 256600山东省滨州市检验检测中心·山东省滨州市化学药物研发与质量控制重点实验室,山东 滨州 256600山东省滨州市检验检测中心·山东省滨州市化学药物研发与质量控制重点实验室,山东 滨州 256600山东省滨州市检验检测中心·山东省滨州市化学药物研发与质量控制重点实验室,山东 滨州 256600山东省滨州市检验检测中心·山东省滨州市化学药物研发与质量控制重点实验室,山东 滨州 256600
医药卫生
小儿四维葡钙片高效液相色谱法超高效液相色谱法葡萄糖蔗糖维生素B1维生素B2维生素C维生素D2含量测定
Xiao'er Siwei Pugai TabletsHPLCUPLCglucosesucrosevitamin B1vitamin B2vitamin Cvitamin D2content determination
《中国药业》 2026 (3)
91-96,6
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