甘油果糖氯化钠注射液含量测定方法的改进

Improved method for the content determination of components in glycerol fructose and sodium chloride injection

目的:对甘油果糖氯化钠注射液中甘油、果糖、氯化钠3种成分的含量测定方法进行改进。方法:采用AgNO_3滴定法测定氯化钠的含量。采用高效液相色谱-示差折光法测定甘油和果糖的含量;色谱条件:使用5u氨基柱(250 mm×4.6 mm,5μm),以乙腈-水(75∶25)为流动相,流速1.0 mL·min^(-1),柱温35℃,流通池温度35℃。结果:氯化钠含量测定滴定终点突跃明显,平均加样回收率(n=9)为99.8%。甘油和果糖进样浓度分别在0.888~4.44和0.488~2.44 mg·mL^(-1)的范围内线性关系良好,检测限(S/N=3)分别为0.042和0.013 mg·mL^(-1),定量限(S/N=10)分别为0.14和0.04 mg·mL^(-1),平均加样回收率(n=9)分别为99.4%和99.5%。10批样品测定结果:氯化钠的含量相对于标示量为98.3%~99.8%,甘油为98.7%~99.6%,果糖为95.2%~96.4%;本方法测定结果与中国药典方法测定结果基本吻合,相对偏差≤1.0%。结论:与中国药典方法相比,本法采用的色谱柱适用面广、便宜易得,待测组分在示差折光检测器上的色谱响应较紫外检测器好。本法可用于甘油果糖氯化钠注射液中甘油、果糖、氯化钠3种成分的含量测定。

Objective： To improve the determination method of the three components （ glycerin, fructose, sodium chloride ） in glycerin fructose and sodium chloride injection. Methods： The content of sodium chloride was determined by silver nitrate titration while glycerol and fructose were determined by HPLC-RID. The chromatographic separation was performed on a 5u NH2 column （ 250 mm × 4.6 mm, 5 μm ） with the mobile phase of acetonitrile-water （ 75 ： 25 ）, the flow rate was 1.0 mL· min-1. The temperature of column and flow cell was set at 35 ℃. Results： The determination method of sodium chloride showed an obvious titration end point and the average recovery was 99.8%. The linear relation was good within the range of 0.888-4.44 mg· mL-1 for glycerol and 0.488-2.44 mg· mL-1 for fructose. LOD （ S/N=3 ）for glycerol and fructose were 0.042 mg· mL-1 and 0.013 mg· mL-1 respectively, while LOQ （ S/N=10 ）were 0.14 mg· mL-land 0.04 mg· mL-1 respectively, and the average recovery for glycerol and fructose were 99.4% and 99.5% respectively. The results from ten batches of samples were as follows： the contents of sodium chloride ranged from 98.3% to 99.8% correspond to labeled amount while glycerol contents ranged from 98.7% to 99.6% and fructose contents ranged from 95.2% to 96.4%. The results were almost the same as those measured by ChP method with the relative deviation less than or equal to 1.0%. Conclusion： Compared with ChP method, the chromatographic column used in this method is cheaper and it can be widely applied. And cheaper and components have better chromatographic behavior detected by differential refractive index detector （ RID ） than those detected by UV detector. The method can be used for quantitative determination of glycerol fructose and sodium chloride injection.