HPLC法和分光光度法测定茴三硫片含量的比较

目的：运用高效液相色谱法和紫外-可见分光光度法对茴三硫片含量进行测定,并对方法学和测定结果进行比较。方法：色谱法中色谱柱Kromasil C18柱（4.6 mm×250 mm,5μm）,以甲醇-水（80∶20）为流动相,检测波长为432 nm;分光光度法于432 nm波长处以外标法测定。结果：HPLC法在32.5～250.0μg/ml浓度范围内其浓度与峰面积呈良好线性关系（r=0.999 9）,平均空白回收率为99.68%（RSD=0.46%,n=9）;分光光度法在4.096～20.480μg/ml浓度范围内其浓度与吸光度呈良好线性关系（r=0.999 4）,平均回收率为99.96%（RSD=0.44%,n=9）;三批样品的平均含量测定结果为：HPLC法分别为99.25%、99.14%和99.10%,分光光度法分别为99.46%、99.22%和99.13%。结论：两种方法均能准确测定茴三硫片的含量,可作为其质量控制的方法。

Comparison of the content assay of Anetholetrithione Tablets determined by HPLC and visible spectrophotometry

Objective：To compare the HPLC and visible spectrophotometry methods in assaying Anetholetrithione Tablets,and the methodology and results were compared respectively.Methods：Kromasil C18（4.6 mm×250 mm,5 μm） was used with mobile phase of methanol-water（80∶20） and the detective wavelength was set at 432 nm in HPLC method;the detective wavelength was set at 432 nm in visible spectrophotometry method.Results：The linear range of anetholtrithione was 32.5-250.0 μg/ml（r=0.999 9）,and the average recovery was 99.68% with RSD 0.46%（n=9） in HPLC method;the visible spectrophotometry method was 4.096-20.480 μg/ml（r=0.999 4）,and the average recovery was 99.96% with RSD 0.44%（n=9）.The average assay results of three batches of samples：HPLC method was 99.25%,99.14% and 99.10%,visible spectrophotometry method was 99.46%,99.22% and 99.13%.Conclusion：Both methods can accurately determine Anetholetrithione Tablets,and can be used as the quality control methods of it.