LC-MS/MS法测定全血中新型安眠药的研究
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摘要
目的建立血液中检测新型安眠药的方法。方法取血液样品过ABN小柱,用甲醇洗脱,洗脱液供LC-MS/MS分析。色谱条件:色谱柱为:kinetex 2.6μC18(50m×3.0mm,2.6μm),以乙腈和水(10 mmol/L甲酸铵)溶液为流动相进行梯度洗脱,进样量为5μL。质谱条件:离子源为ESI源;监测方式为正离子多离子反应监测(MRM);扫描范围分别为全扫描。结果唑吡坦、扎来普隆和氟硝西泮的线性范围为1～500ng/mL,佐匹克隆、氯硝西泮和diclaepam的线性范围为5～500ng/mL,7-氨基氯硝西泮和尼美西泮的线性范围为1～250ng/mL,地洛西泮和氯甲西泮的线性范围为5～250ng/mL;日内精密度和日间精密度均≤15%(n=5);回收率范围为53.6-101.3%;基质效应范围为63.64-118.0%。结论该方法专属性强、灵敏度高、简单快速可用于新型安眠药的检测。
Objectives To establish the method for the determination of new hypnotics. Method Take a blood sample over the ABN column, then elute it with methanol for the analysis by HPLC-MS/MS. Chromatographic condition: the determination was performed on a kinetex column 2.6μC18(50 m×3.0 mm) and eluted with acetonitrile water containing 10 mmol/L ammonium formate in a gradient program. The injection volume was 5μL. Mass spectrum condition: The ion source is ESI source. The multiple-reaction monitoring scanning(MRM) was performed for the determination with switching electrospray ion source polarity in positive mode. The scanning scope was the whole scan. Results The linear ranges were 1～500 ng/mL for zolpidem,zaleplon and fluitrazpam, 5～500 ng/mL for zopiclone,clonazepam and diclazepam,1～250 ng/mL for 7-Aminoclonazepam and nimetazepam and 5～250 ng/mL for delorazepam and lormetazepam; The recovery range was 53.65-101.3%. the matrix effects range was 63.64-118.0%. The intra-day and inter-day precision were both less than 15%(n=5). Conclusion The method is simple, rapid, and sensitive. It could be employed as a determination method for new hypnotics.
Objectives To establish the method for the determination of new hypnotics. Method Take a blood sample over the ABN column, then elute it with methanol for the analysis by HPLC-MS/MS. Chromatographic condition: the determination was performed on a kinetex column 2.6μC18(50 m×3.0 mm) and eluted with acetonitrile water containing 10 mmol/L ammonium formate in a gradient program. The injection volume was 5μL. Mass spectrum condition: The ion source is ESI source. The multiple-reaction monitoring scanning(MRM) was performed for the determination with switching electrospray ion source polarity in positive mode. The scanning scope was the whole scan. Results The linear ranges were 1～500 ng/mL for zolpidem,zaleplon and fluitrazpam, 5～500 ng/mL for zopiclone,clonazepam and diclazepam,1～250 ng/mL for 7-Aminoclonazepam and nimetazepam and 5～250 ng/mL for delorazepam and lormetazepam; The recovery range was 53.65-101.3%. the matrix effects range was 63.64-118.0%. The intra-day and inter-day precision were both less than 15%(n=5). Conclusion The method is simple, rapid, and sensitive. It could be employed as a determination method for new hypnotics.
引文
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[2]李贤良,严爱花,郗存显,等.液相色谱-串联质谱法同时检测牛奶中20种苯二氮卓类药物残留[J].分析实验室,2013,32(4):42-47.
[3]郭琦,石银涛,王绘军.血液中佐匹克隆自动固相萃取-液相色谱-飞行时间质谱法定性与确证方法研究[J].分析实验室,2014,33(9):1055-1058.
[4]王朝虹,张琳,赵蒙.超高效液相色谱-质谱定量测定全血中的13种苯二氮卓类安眠镇静药物[J].刑事技术,2016,41(1):46-49.
[5]王丽梅.固相萃取-HPLC法快速测定四种常用镇静催眠药的血药浓度[J].临床医药实践杂志,2004,13(4):303-304.
[6]孙剑聪,杨帆.麻醉抢劫案件血液及牛奶类饮料中常见安眠镇静药物的SPE-GC-MS快速分析方法[J].技术应用,2013,22(22):107-108.
[2]李贤良,严爱花,郗存显,等.液相色谱-串联质谱法同时检测牛奶中20种苯二氮卓类药物残留[J].分析实验室,2013,32(4):42-47.
[3]郭琦,石银涛,王绘军.血液中佐匹克隆自动固相萃取-液相色谱-飞行时间质谱法定性与确证方法研究[J].分析实验室,2014,33(9):1055-1058.
[4]王朝虹,张琳,赵蒙.超高效液相色谱-质谱定量测定全血中的13种苯二氮卓类安眠镇静药物[J].刑事技术,2016,41(1):46-49.
[5]王丽梅.固相萃取-HPLC法快速测定四种常用镇静催眠药的血药浓度[J].临床医药实践杂志,2004,13(4):303-304.
[6]孙剑聪,杨帆.麻醉抢劫案件血液及牛奶类饮料中常见安眠镇静药物的SPE-GC-MS快速分析方法[J].技术应用,2013,22(22):107-108.