Simultaneous Determination of Six Residual Solvents in Phenylbutazone Raw Material by Head-space GC
- VernacularTitle:顶空气相色谱法同时测定保泰松原料药中6种溶剂残留量
- Author:
Xiru ZHANG
1
;
Ting SUN
1
;
Chen WANG
1
;
Yun LIU
2
Author Information
1. Hebei Institute for Drug Control，Shijiazhuang 050011，China
2. Shijia zhuang Center for Food and Drug Control，Shijiazhuang 050011，China
- Publication Type:Journal Article
- Keywords:
Phenylbutazone raw material;
Head-space GC;
Residual solvent;
Methanol;
Ethanol;
Isopropyl alcohol;
Dichloromethane;
Ethyl acetate;
N， N-dimethyl formamide
- From:
China Pharmacy
2019;30(6):780-784
- CountryChina
- Language:Chinese
-
Abstract:
OBJECTIVE： To establish a method for simultaneous determination of residual solvents in phenylbutazone raw material. METHODS： Head-space GC was adopted. The determination was performed on Agilent HP-5 capillary column by temperature programming. The temperature of injector was 200 ℃， and detector was flame ionization detector with temperature of 250 ℃； carrier gas was nitrogen （purity：99.99％） at the flow rate of 2.0 mL/min. The split ratio was 5 ∶ 1. Headspace equilibrium temperature was 60 ℃， and equilibration time was 30 min. The sample size was 1 mL. RESULTS： The linear range was 0.15-4.5 μg/mL for methanol （r＝0.999 9）， 0.25-7.5 μg/mL for ethanol （r＝0.999 7）， 0.25-7.5 μg/mL for isopropyl alcohol （r＝0.999 7）， 0.03-0.9 μg/mL for dichloromethane （r＝0.999 3）， 0.25-7.5 μg/mL for ethyl acetate （r＝0.999 3）， 0.044-1.32 μg/mL for N，N-dimethyl formamide （r＝0.999 3）， respectively. The limits of detection were 0.05， 0.08， 0.08， 0.01， 0.08， 0.015 μg/mL. The limits of quantitation were 0.15， 0.25， 0.25， 0.03， 0.25， 0.044 μg/mL. RSDs of precision test were lower than 2.0％. RSDs of stability and reproducibility tests were lower than 3.0％. The recoveries were 98.75％-100.12％ （RSD＝0.56％， n＝9）， 98.07％-101.20％ （RSD＝1.12％， n＝9）， 98.36％-100.80％ （RSD＝0.92％， n＝9）， 98.33％-101.67％ （RSD＝0.98％， n＝9）， 98.11％-100.40％ （RSD＝0.72％， n＝9） and 98.75％-101.05％ （RSD＝0.89％， n＝9）. CONCLUSIONS： The method is simple， accurate， precise， stable， reproducible and durable， and can be used for simultaneous determination of 6 residual solvents in phenylbutazone raw material.
