柱前衍生化顶空进样气相色谱法测定蚂蚁及其制剂中蚁酸的含量  

Determination of formic acid in ants and their preparations by gas chromatography with pre⁃column derivatization and headspace injection

作　　者：梁卜文 申国华 董培智 LIANG Buwen;SHEN Guohua;DONG Peizhi(Institute of Drug Inspection Technology,Shanxi Provincial Inspection and Testing Center,Key Laboratory of Food and Drug Safety Prevention and Control,Taiyuan 030031,China)

机构地区：[1]山西省检验检测中心药品检验技术研究所,食品药品安全防控山西省重点实验室,太原030031

出　　处：《山西医科大学学报》2025年第2期175-181,共7页Journal of Shanxi Medical University

基　　金：食品药品安全防控山西省重点实验室基金资助项目(202204010931006)。

摘　　要：目的 建立测定蚂蚁及其制剂中蚁酸的含量测定方法。方法 采用气相色谱法(GC)检测蚂蚁及其制剂中蚁酸的含量。蚁酸与异丙醇经过酯化反应生成甲酸异丙酯,采用顶空的进样方式,以氢火焰离子化检测器(FID)为检测器,85℃平衡30 min,顶空进样。色谱分离条件为:柱箱初始温度50℃,程序升温20℃/min,色谱柱载气流量2.5 mL/min,分流比10∶1。对建立的顶空进样气相色谱法进行方法学考察。结果 蚁酸在20~600μg之间线性关系良好(R^(2)=0.999 2),平均回收率95.2%~95.9%,中间精密度RSD为2.0%,重复性RSD为2.9%,检出限为0.007 0 mg/g,定量限为0.020 mg/g。结论 本方法快速、简便、准确,适用于蚂蚁及其制剂中蚁酸的含量测定。Objective To establish a method for determining the content of formic acid in ants and their preparations.Methods The content of formic acid in ants and their preparations was determined by gas chromatography(GC).Formic acid and isopropanol were esterified to form isopropyl formate.The headspace injection method was adopted,with FID(hydrogen flame ionization detector)as the detector,85℃equilibrated for 30 min,and headspace injection.The chromatographic separation conditions were as follows:the initial temperature of the column was 50℃,the program temperature ramping rate was 20℃/min,the carrier gas flow rate of the chromatographic column was 2.5 mL/min,and the split ratio was 10∶1.The methodology of the established headspace injection gas chromatography method was investigated.Results Formic acid had a good linear relationship in the range of 20-600μg(R^(2)=0.9992),the average recovery rate was 95.2%-95.9%,the intermediate precision RSD was 2.0%,the repeatability RSD was 2.9%,the detec-tion limit was 0.0070 mg/g,and the quantification limit was 0.020 mg/g.Conclusion This method is rapid,simple and accurate,and it is suitable for the determination of formic acid in ants and their preparations.

关 键 词：蚁酸 蚂蚁制剂 柱前衍生化 顶空进样 气相色谱法 含量测定 方法学验证 

分 类 号：R927[医药卫生—药学]