现代仪器与医疗
現代儀器與醫療
현대의기여의료
Modern Instrument and Medical Treatment
2015年
1期
61-63
,共3页
商国举%全红娜%蔡振华%蒋庆峰
商國舉%全紅娜%蔡振華%蔣慶峰
상국거%전홍나%채진화%장경봉
硫酸氢氯吡格雷%残留溶剂%气相色谱法
硫痠氫氯吡格雷%殘留溶劑%氣相色譜法
류산경록필격뢰%잔류용제%기상색보법
Clopidogrel Bisulfate%residual solvents%gas chromatography
目的：建立顶空气相色谱法,测定硫酸氢氯吡格雷中丙酮、异丙醇、乙腈、二氯甲烷和乙酸乙酯5种残留溶剂方法。方法：采用D B-624（6%-氰丙基苯-94%-二甲基硅氧烷共聚物，30m ×0.53m m , d f=3.0μ m）毛细管柱，检测器：F I D；温度：250℃；气化室温度：220℃；载气：氮气；流速：4.0m L/m i n；程序升温：40℃，保持8m i n，以80℃/m i n的速度升至200℃保持3m i n。结果：此色谱条件下，5种溶剂均能得到良好的分离，空白对照无干扰。丙酮、异丙醇和乙酸乙酯在浓度0.25～0.7250mg/mL（r=0.9999、r=0.9985、r=0.9976）范围内，二氯甲烷在浓度0.03～0.0870mg/mL（r=0.9989）范围内，乙腈在浓度0.0205～0.0595mg/mL（r=0.9965）范围内，线性关系良好。平均回收率（n=9）分别为丙酮99.57%（R S D=3.86%）、异丙醇100.03%（R S D=4.38%）、乙腈105.11%（RSD=3.32%）、二氯甲烷99.99%（RSD=3.01%）、乙酸乙酯99.71%（RSD=3.19%）。结论：方法测定结果准确，灵敏简便，可有效检测硫酸氢氯吡格雷中有机溶剂残留量。
目的：建立頂空氣相色譜法,測定硫痠氫氯吡格雷中丙酮、異丙醇、乙腈、二氯甲烷和乙痠乙酯5種殘留溶劑方法。方法：採用D B-624（6%-氰丙基苯-94%-二甲基硅氧烷共聚物，30m ×0.53m m , d f=3.0μ m）毛細管柱，檢測器：F I D；溫度：250℃；氣化室溫度：220℃；載氣：氮氣；流速：4.0m L/m i n；程序升溫：40℃，保持8m i n，以80℃/m i n的速度升至200℃保持3m i n。結果：此色譜條件下，5種溶劑均能得到良好的分離，空白對照無榦擾。丙酮、異丙醇和乙痠乙酯在濃度0.25～0.7250mg/mL（r=0.9999、r=0.9985、r=0.9976）範圍內，二氯甲烷在濃度0.03～0.0870mg/mL（r=0.9989）範圍內，乙腈在濃度0.0205～0.0595mg/mL（r=0.9965）範圍內，線性關繫良好。平均迴收率（n=9）分彆為丙酮99.57%（R S D=3.86%）、異丙醇100.03%（R S D=4.38%）、乙腈105.11%（RSD=3.32%）、二氯甲烷99.99%（RSD=3.01%）、乙痠乙酯99.71%（RSD=3.19%）。結論：方法測定結果準確，靈敏簡便，可有效檢測硫痠氫氯吡格雷中有機溶劑殘留量。
목적：건립정공기상색보법,측정류산경록필격뢰중병동、이병순、을정、이록갑완화을산을지5충잔류용제방법。방법：채용D B-624（6%-청병기분-94%-이갑기규양완공취물，30m ×0.53m m , d f=3.0μ m）모세관주，검측기：F I D；온도：250℃；기화실온도：220℃；재기：담기；류속：4.0m L/m i n；정서승온：40℃，보지8m i n，이80℃/m i n적속도승지200℃보지3m i n。결과：차색보조건하，5충용제균능득도량호적분리，공백대조무간우。병동、이병순화을산을지재농도0.25～0.7250mg/mL（r=0.9999、r=0.9985、r=0.9976）범위내，이록갑완재농도0.03～0.0870mg/mL（r=0.9989）범위내，을정재농도0.0205～0.0595mg/mL（r=0.9965）범위내，선성관계량호。평균회수솔（n=9）분별위병동99.57%（R S D=3.86%）、이병순100.03%（R S D=4.38%）、을정105.11%（RSD=3.32%）、이록갑완99.99%（RSD=3.01%）、을산을지99.71%（RSD=3.19%）。결론：방법측정결과준학，령민간편，가유효검측류산경록필격뢰중유궤용제잔류량。
Objective: To establish a method of headspace gas chromatography for the determination of ifve organic residual solvents (acetone, isopropanol, acetonitrile, methylene chloride and ethyl acetate) in Clopidogrel Bisulfate.Methods:A capillary GC method was established with FID detector, using the DB-624 (6%-94% cyanide propylbenzene-dimethylsiloxane copolymer, 30m×0.53mm, df=3.0μm) capillary column. The injector temperature and the detector temperature were controlled at 220℃ and 250℃ respectively. The carried gas was N2, the lfow rate was 4.0mL/min. The column temperature is initially maintained at 40℃ for 8min and then up to 200℃ at the rate of 80℃/min for 3min.Results: The detected ifve solvents were separated completely, blank control had no interference. The peak area and concentration of acetone, isopropyl alcohol and ethyl acetate showed a good linearity within the concentration range of 0.25~0.7250mg/mL (r=0.9999、r=0.9985、r=0.9976. The peak area and concentration of methylene chloride showed a good linearity within the concentration range of 0.03~0.0870mg/mL (r=0.9989) the peak area and concentration of acetonitrile showed a good linearity within the concentration range of 0.0205~0.0595mg/mL (r=0.9965). The average recovery of acetone, isopropanol, acetonitrile, methylene chloride, ethyl acetate was calculated as 99.57% (RSD=3.86%), 100.03% (RSD=4.38%), 105.11% (RSD=3.32%), 99.99% (RSD=3.01%), 99.71% (RSD=3.19%) respectively (n=9).Conclusion: This method is accurate, sensitive and simple, and can be effectively used in the determination of residual organic solvents in Clopidogrel Bisulfate.
