1.公安部物证鉴定中心,北京 100038
2.爱博才思亚太应用支持中心,北京 100015
张云峰,硕士,副研究员,研究方向:毒物分析,E-mail:yunfeng_2002@sohu.com
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赵鹏,常靖,吴小军等.超高效液相色谱-串联质谱检测干血斑中29种β2-受体激动剂[J].分析测试学报,2022,41(02):227-233.
ZHAO Peng,CHANG Jing,WU Xiao-jun,et al.Determination of 29 β2-agonists in Dried Blood Spots by Ultra-high Performance Liquid Chromatography-Tandem Mass Spectrometry[J].Journal of Instrumental Analysis,2022,41(02):227-233.
赵鹏,常靖,吴小军等.超高效液相色谱-串联质谱检测干血斑中29种β2-受体激动剂[J].分析测试学报,2022,41(02):227-233. DOI: 10.19969/j.fxcsxb.21040103.
ZHAO Peng,CHANG Jing,WU Xiao-jun,et al.Determination of 29 β2-agonists in Dried Blood Spots by Ultra-high Performance Liquid Chromatography-Tandem Mass Spectrometry[J].Journal of Instrumental Analysis,2022,41(02):227-233. DOI: 10.19969/j.fxcsxb.21040103.
该研究建立了干血斑中29种,β,2,-受体激动剂的超高效液相色谱-串联质谱(UPLC-MS/MS)检测方法,分别对流动相、干血斑提取溶剂种类及比例进行了优化。采用甲醇对干血斑进行提取,Phenomenex Kinetex F5(3.0 mm × 100 mm,2.6 μm)色谱柱进行分离,以1 mmol/L甲酸铵-0.01%甲酸水溶液和乙腈作为流动相进行梯度洗脱,提取液直接进行UPLC-MS/MS分析。结果表明,干血斑中29种,β,2,-受体激动剂在一定的质量浓度范围内线性关系良好,相关系数(,r,2,)为0.995 8~0.999 9,方法检出限(LOD)为1~10 ng·mL,-1,;除非诺特罗外,其余化合物的加标回收率为60.9%~124%,相对标准偏差(RSD)均小于10%。制备的干血斑样品在-20 ℃冰箱保存8周后,干血斑中化合物的稳定性与全血加标样品相比无明显变化。该方法简单准确,样品用量小,且保存和运输便利,可为法庭毒物分析提供新的方法和思路。
A large number of ,β,2,-agonist poisoning or death cases have been reported. It is urgent to establish a toxicological assay for ,β,2,-agonist poisoning in blood applicable to forensic toxicology analysis since the current methods for ,β,2,-agonists detection mainly focus on the edible tissues of animal products or the illegal addition of drugs.Compared with traditional whole blood collection techniques,the dried blood spots(DBSs) offers several advantages. It is a simple and minimally invasive sample collection technique,involving collecting a small sample volume,easy to transport and store.In recent years,the DBSs have been gradually applied to drug metabolism and toxicological analysis,and a large number of quantitative methods for the detection of drug abuse and psychoactive substances have been reported.An ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS) was developed for the qualitative and quantitative determination of 29 ,β,2,-agonists in dried blood spots in this paper.The mobile phase,type and proportion of extraction solvents were optimized. Stability of 29 ,β,2,-agonists in the DBS sample was investigated. The DBSs were firstly extracted with methanol, then separated on a Phenomenex Kinetex F5(3.0 mm × 100 mm,2.6 μm) column,with 1 mmol/L ammonium formate-0.01% formic acid aqueous solution and acetonitrile as mobile phases,and finally analyzed by UPLC-MS/MS.Results showed that there were good relationships for 29 ,β,2,-agonists in DBSs in a certain concentration range, with their correlation coefficients(,r,2,) of 0.995 8-0.999 9 and limits of detection(LOD) of 1-10 ng·mL,-1,. The spiked recoveries for 28 ,β,2,-agonists were in the range of 60.9%-124% except fenoterol,with relative standard deviations(RSD) less than 20%.The analytes in DBSs stored at -20 ℃ for 8 weeks showed the same stability as those of the whole blood sample.The method was accurate and simple,and was convenient to storage and transport.It provided a new method and thought for forensic toxicological analysis.
β2-受体激动剂干血斑法庭毒物分析超高效液相色谱-串联质谱(UPLC-MS/MS)
β2-agonistsdried blood spotsforensic toxicological analysisultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)
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