HPLC-MS/MS法检测2-氯-2-脱氧-D-葡萄糖方法优化及验证
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摘要
建立了高效液相色谱-三重四极杆串联质谱(HPLC-MS/MS)检测2-氯-2-脱氧-D-葡萄糖(ClDG)的分析方法。采用多反应监测(MRM)负离子电喷雾模式进行HPLC-MS/MS分析。色谱柱为:Alltima Amino 100A 5μm柱(250 mm×4.6 mm),流动相为:V(5 mmol/L乙酸铵)∶V(乙腈)=10∶90;柱温:35℃;流速:1 mL/min;进样量:5μL。ClDG浓度在0.5~37.5μg/m L范围内与峰面积有良好的线性关系,检出限为0.15μg/mL,定量限为0.5μg/mL,方法回收率为92.6%~105.1%。该方法选择性、重复性良好,灵敏度高,能用于ClDG的痕量分析。
A method for the determination of 2-chloro-2-deoxy-D-glucose(ClDG) by high performance liquid chromatography-triple quadrupole mass spectrometry(HPLC-MS/MS) was established. HPLC-MS/MS analysis was performed using multiple reaction monitoring(MRM) negative ion electrospray mode.The column was: Alltima Amino 100 A 5 μm(250 mm×4. 6 mm),mobile phase: 5 mmol/L ammonium acetate-acetonitrile(10 ∶ 90); column temperature: 35 ℃; flow rate: 1 mL/min; injection volume:5 μL.There was a good linear relationship between the concentration of ClDG and the peak area in the range of 0. 5 to 37. 5μg/mL.The detection limit was 0. 15 μg/mL and the limit of quantitation was 0. 5 μg/mL. The recovery of the method was92. 6% ~ 105. 1%.The method has good selectivity,good repeatability and high sensitivity and can be used for the trace analysis of2-chloro-2-deoxy-D-glucose(ClDG).
A method for the determination of 2-chloro-2-deoxy-D-glucose(ClDG) by high performance liquid chromatography-triple quadrupole mass spectrometry(HPLC-MS/MS) was established. HPLC-MS/MS analysis was performed using multiple reaction monitoring(MRM) negative ion electrospray mode.The column was: Alltima Amino 100 A 5 μm(250 mm×4. 6 mm),mobile phase: 5 mmol/L ammonium acetate-acetonitrile(10 ∶ 90); column temperature: 35 ℃; flow rate: 1 mL/min; injection volume:5 μL.There was a good linear relationship between the concentration of ClDG and the peak area in the range of 0. 5 to 37. 5μg/mL.The detection limit was 0. 15 μg/mL and the limit of quantitation was 0. 5 μg/mL. The recovery of the method was92. 6% ~ 105. 1%.The method has good selectivity,good repeatability and high sensitivity and can be used for the trace analysis of2-chloro-2-deoxy-D-glucose(ClDG).
引文
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[2]CRIPPA S,SALGARELLO M.The role of 18fluoro-deoxyglucose positron emission tomography computed tomography in resectable pancreatic cancer[J].Dig.Liver Dis.,2014,46(8):744-749.
[3]FARN S S,YEH Y H.Development and validation of 2-deoxy-2-chloro-D-glucose impurity analysis in[18F]FDG by three potential-time waveforms of high-performance liquid chromatography/pulsed amperometric detection[J].Nucl.Med.Biol.,2009,36(2):225-231.
[4]NAKAO R,KIDA T.Factors affecting quality control of[18F]FDG injection:bacterial endotoxins test,aluminum ions test and HPLC analysis for FDG and CIDG[J].Appl.Radiat.Isotopes,2005,62(6):889-895.
[5]CHAAR M R,DUFEK P.Identification of 2-chloro-2-deoxyglucose(2-CIDG)and D-glucose as impurities formed in the synthesis of 2-[18F]Fluoro-2-deoxyglucose(2-18FDG)[J].Appl.Radiat.Isotopes,1994,2(45):267-270.
[6]袁艳娟,刘晶,乔红群.HPLC-MS法检测氟[18F]脱氧葡萄糖([18F]-FDG)注射液中2-氯-2-脱氧-D-葡萄糖(Cl DG)的含量[J].分析试验室,2012,31(5):93-95.
[7]张强,谢新民.高效液相-蒸发光散射法检测氟[18F]脱氧葡糖注射液中2-氯-2-脱氧-D-葡萄糖含量[J].中国药业,2016,25(12):69-71.
[8]NAKAO R,ITO T,YAMAGUCHI M,et al.Simultaneous analysis of FDG,Cl DG and Kryptofix 2.2.2 in[18F]FDG preparation by high-performance liquid chromatography with UV detection[J].Nucl.Med.Biol.,2008,35(2):239-244.
[9]ALEXOFF D L,CASATI R.Ion chromatographic analysis of high specific activity 18FDG preparations and detection of the chemical impurity 2-deoxy-2-chloro-D-glucose[J].Appl.Radiat.Isotopes,1992,43(11):1 313-1 322.