Objective: To establish a headspace gas chromatography method that can simultaneously determine the residues of vinylidene chloride, 1,1-dichloroethane and 1,2-dichloroethane in medicinal composite hard tablets. Methods: Equilibrate the headspace vial at 80 ℃, for 20 min. The sample inlet temperature was 220 ℃, and the split ratio was 10∶1. DB-624 column (30 m×0.32 mm, 1.8 μm)was used with high-purity nitrogen (purity 99.999%) as the carrier gas. The flow rate was 1.0 mL·min-1. The column temperature was maintained at 35 ℃ for 8 min, increased to 70 ℃ at 20 ℃·min-1 for 3 min, and then increased to 220 ℃ at 100 ℃·min-1 for 5 min. The FID detector temperature was 250 ℃. Results: The linear ranges of vinylidene chloride, 1,1-dichloroethane and 1,2-dichloroethane were 0.06-4 μg (r=0.996 8)、0.015-6 μg(r=0.999 1) and 0.006-2.4 μg(r=0.999 4), respectively. The recoveries were 104.2%, 102.2% and 96.2% respectively, and the precisions were 3.4%, 5.2% and 4.5% respectively. Conclusion: The method is simple, accurate, sensitive and reproducible. It can be used for the determination of vinylidene chloride, 1, 1-dichloroethane and 1, 2-dichloroethane residues in medicinal composite hard tablets.
FENG Yu-wei, WU Hong-yang, CAO Xi, FAN Neng-quan
. Determination of vinylidene chloride, 1, 1-dichloroethane and 1,2-dichloroethane in medicinal composite hard tablets[J]. Chinese Journal of Pharmaceutical Analysis, 2022
, 42(12)
: 2163
-2168
.
DOI: 10.16155/j.0254-1793.2022.12.13
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