顶空进样气相色谱法筛选并测定脉络宁注射液中有机溶剂残留量

 目的 筛选脉络宁注射液中残留有机溶剂，并建立方法测定其残留量，为质量评价提供依据。方法 采用顶空进样气相色谱法，以键合聚乙二醇（HP-INNOWAX毛细管柱和5%二苯基-95%二甲基硅氧烷共聚物（HP-5毛细管柱相互验证进行筛选，以HP-5进行测定，载气N₂，流速4.0 mL·min-1，恒流方式；柱升温程序：起始柱温50 ℃；保持5 min，以10 ℃·min-1升温至150 ℃；进样口温度150 ℃；检测器（FID温度250 ℃；尾吹（N₂30 mL·min-1。顶空进样1 mL，分流比1∶1。顶空进样瓶平衡温度85 ℃，平衡时间20 min，传输管温度110 ℃，进样环温度105 ℃。结果 79批脉络宁注射液中筛查出4种溶剂，乙酸乙酯在14批样品中未检出，其余65批中为0.000 01%～0.000 7%，乙醇为0.004%～0.049%，甲醇为0.004%～0.018%，丙酮为0.000 3%～0.002 7%。4种溶剂在0.000 79～4.5 mg·mL-1内线性关系良好，r均为1.000 0(n=7；检测限为0.032～0.079 ng·mL-1，定量限为0.090～0.198 ng·mL-1；日内精密度小于3.0%(n=6，日间精密度小于9.1%(n=3；平均回收率为92.0%～110.9%(RSD为2.2%～5.7% ，n=6。结论 所建立的方法准确、快速、灵敏，测定结果较全面地反映了脉络宁注射液中有机溶剂残留量状况，为其质量评价提供了依据。

Screening and Analyses on the Residues of Organic Solvents in Mailuoning Injection by GC with Headspace Sampler

OBJECTIVE To develop a method for analyzing on organic solvent residues in Mailuoning Injection， based on screening multi residues of solvents， in order to give the quality evaluation of the injection. METHODS GC instrument coupled with headspace sampler was used. The separation were carried out on HP-5 column， based on screening results of dual columns of HP-INNOWAX and HP-5. A nitrogen flow rate was set at 4.0 mL·min-1 in a constant flow mode， using an oven temperature program from 50 ℃(5 min to 150 ℃ at a rate of 10 ℃·min-1. Injection inlet was 150 ℃ and FID was 250 ℃ and the make up was 30 mL·min-1. 1 mL was injected by headspace sampler in the split mode with the split ratio of 1∶1. The headspace vials were balanced at 85 ℃ for 20 min， the transfer line and sampling loop were set at 110 ℃ and 105 ℃， respectively. RESULTS Ethyl acetate was undetected in 14 batches of samples and 0.000 01%-0.000 7% in 65 batches， ethanol， methanol and acetone fell in the range of 0.004%-0.049%， 0.004%-0.018% and 0.000 3%-0.002 7%， respectively. A good linear behavior was indicated by r value of 1.000 0(n=7in the concentration rang from 0.000 79 to 4.5 mg·mL-1. The LODs and LOQs were 0.032-0.079 and 0.090-0.198 ng·mL-1， and inter-day and intra-day precisions were below 3.0%(n=6and 9.1%(n=3， respectively. The average recoveries were in the range from 92.0% to 110.9%， with RSDs of 2.2%-5.7%(n=6. CONCLUSION The developed method is accurate， rapid and sensitive. The results could provide a survey of the residues of organic solvents in Mailuoning Injection and a reference to the quality evaluation of the injection.