目的 采用高效液相-蒸发光散射检测法(HPLC-ELSD)测定不同厂家清开灵注射液中木糖、果糖、葡萄糖和蔗糖的含量,并根据4种糖的含量水平对8个厂家的产品进行聚类分析。方法 采用Prevail Carbohydrate ES糖分析色谱柱(4.6 mm × 250 mm, 5 μm),乙腈(B)-水(A)为流动相,线性梯度洗脱,流速为1.0 mL·min-1,柱温为30 ℃;ELSD检测器:漂移管温度为90.7 ℃,雾化气(空气)流速为2.4 L·min-1,测定清开灵注射液中4种糖的含量,并利用SPSS 16.0进行聚类分析。结果 4种糖在色谱柱上分离效果良好,并具有良好的线性范围;木糖、果糖、葡萄糖、蔗糖的平均加样回收率分别为98.52% (RSD=1.70%)、99.15% (RSD=2.55%)、99.82% (RSD=2.04%)、99.26% (RSD=1.67%);聚类分析将不同厂家清开灵样品分成3类。结论 该方法简便、稳定、重复性好,可用于清开灵注射液中糖类成分测定,并为其质量控制提供理论依据。
Abstract
ObjectiveTo establish an HPLC-ELSD method to determine the contents of four saccharides in Qingkailing injection and carry out cluster analysis of the products from different manufactures. Methods Chromatographic separation was performed on a Prevail Carbohydrate ES column with mobile phase of acetonitrile (B) - water (A) at a flow rate of 1.0 mL·min-1 with gradient elution; the column temperature was 30 ℃; the ELSD drift tube temperature was 90.7 ℃ and the gas flow was 2.4 L·min-1. Cluster analysis was performed by SPSS16.0. Results Good resolution and linearities were obtained. The average recoveries of xylose, fructose, glucose and sucrose were 98.52% (RSD=1.70%), 99.15% (RSD=2.55%), 99.82% (RSD=2.04%) and 99.26% (RSD=1.67%), respectively. The test samples were clustered into three classes. Conclusion The established method is simple, reliable and accurate. It can be used to determine the saccharide components in Qingkailing injection, and provide theoretical basis for its quality control.
关键词
高效液相-蒸发光散射检测法 /
清开灵注射液 /
聚类分析 /
木糖 /
果糖 /
葡萄糖 /
蔗糖
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Key words
HPLC-ELSD /
Qingkailing injection /
cluster analysis /
xylose /
fructose /
glucose /
sucrose
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中图分类号:
R917
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脚注
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基金
基金项目:国家重大新药创制专项资助项目(2010ZX09502-002)
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