气相色谱法测定静注人免疫球蛋白(10%)辛酸钠残留量  

Determination of residual sodium octanoate in human immunoglobulin(10%)by gas chromatography

作　　者：贺丽娟 陈通威 申云飞 路海滨[2] HE Li-juan;CHEN Tong-wei;SHEN Yun-fei;LU Hai-bin(Shanxi Kangbao Biological Product Co.,Ltd.,Changzhi 046000,China;School of Pharmaceutical Sciences Jilin University,Changchun 130012,China)

机构地区：[1]山西康宝生物制品股份有限公司,长治046000 [2]吉林大学药学院,长春130012

出　　处：《药物分析杂志》2023年第9期1507-1513,共7页Chinese Journal of Pharmaceutical Analysis

基　　金：山西省重点研发计划项目资助(202102130501019)。

摘　　要：目的:建立静注人免疫球蛋白(10%)中辛酸钠残留量毛细管气相色谱测定法。方法:采用ZB-FFAP毛细管柱(15 m×0.53 mm×1.0μm),柱温160℃,气化室温度230℃,载气为氮气,以氢火焰检测器(FID检测器)测定,检测器温度230℃,流速8 mL·min^(-1),分流比为23∶1,进样体积1μL,内标法定量,庚酸为内标物。结果:供试3批样品中均未检出辛酸钠残留;辛酸峰和庚酸峰的分离度>1.5,辛酸峰的拖尾因子在0.95~1.20;辛酸对照品溶液连续进样5次,所得辛酸峰与庚酸峰面积之比的RSD<5%;配制的空白基质经检测对辛酸峰和庚酸峰均无影响;辛酸量在100~300μg范围内线性良好,相关系数(r)大于0.99;方法检测限为0.010 mg·mL^(-1),定量限为0.033 mg·mL^(-1);高、中、低3种不同浓度样品加标平均回收率为100.1%;温度的高低只影响主峰和内标峰的保留时间,不影响实验结果。结论:本实验建立的分析方法分离度好,操作过程简便,方法灵敏,环境友好,结果准确,重现性好,可用于静注人免疫球蛋白(10%)辛酸钠残留的测定。Objective: To establish a capillary gas chromatography method for the determination of sodium octanoate residues in intravenous human immunoglobulin(10%). Methods: ZB-FFAP capillary column(15 m×0.53 mm×1.0 μm) was adopted, the column temperature was 160 ℃, the gasification chamber temperature was 230 ℃. Nitrogen was used as the carrying gas. Hydrogen flame detector(FID) was used and the detector temperature was 230 ℃. The flow rate was 8 mL·min^(-1), the split ratio was 23∶1 and the sample volume was 1 μL. Heptanoic acid were used as the internal standard. Results: No sodium octanoate residue was detected in three batches of samples. The resolution between octanoic acid peak and heptanoic acid peak were higher than 1.5. The trailing factor of octanoic acid peak was between 0.95 and 1.20. Octanoic acid standard solution was injected for 5 times, RSD of the ratio between the peak area of octanoic acid and heptanoic acid was less than 5%. Blank matrix had no effect on the peak of octanoic acid and heptanoic acid. Linearity of octanoic acid in the range of100-300 μg was good and correlation coefficient(r) was greater than 0.99. The limits of detection and quantification were 0.010 mg·mL^(-1) and 0.033 mg·mL^(-1), respectively. The average recovery of three different concentrations of samples was 100.1%. The retention time of main peak and internal standard peak was only affected by increasing and decreasing the temperature respectively, and the experimental results were stable. Conclusion: The method established in this study was simple, sensitivity and environmentally friendly. The results were accurate and reproducible. The method can be used for the determination of sodium octanoate residue in intravenous human immunoglobulin(10%).

关 键 词：静注人免疫球蛋白 辛酸钠 残留量 毛细管气相色谱法 内标法 辛酸 庚酸 

分 类 号：R917[医药卫生—药物分析学]