血液中甲卡西酮法医学检测方法的建立及应用
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摘要
目的建立血液中甲卡西酮法医学检测方法。方法在含有甲卡西酮的血液中,加入内标双苯戊二氨酯(SKF525A),加氢氧化钠溶液调节pH> 12,用乙酸乙酯提取,提取液在50℃氮气流下挥干,用甲醇溶解残余物,用GC-MS分析。GC-MS条件:HP-5MS(30 m×0.25 mm×0.25μm)石英毛细管柱;柱温:初温60℃保持1.5 min,以10℃·min~(-1)速率升温至200℃保持10 min,以5℃·min~(-1)速率升温至250℃保持5 min;接口温度280℃;离子源:EI源,温度230℃;四极杆温度:150℃;扫描方式:SCAN 40～450 amu,SIM甲卡西酮m/z 58、77、105,SKF525 A m/z 86、99、165。结果甲卡西酮在20～2000 ng·mL~(-1)内与峰面积线性关系良好,线性方程为y=0.3053×10~(-3)x+0.0112(r=0.999),检出限为10 ng·mL~(-1)。添加浓度为100～1000 ng·m L~(-1)时,平均相对回收率为92.6%～98.9%,绝对回收率为81.6%～86.6%,RSD为6.5%～8.9%(n=5),日内和日间精密度在7.0%～8.8%。结论该方法操作简便、检测灵敏度较高,可应用于涉毒案件血液中甲卡西酮的测定。
Objective To develope a forensic method to determine methcathinone in the blood. Methods Proadifen hydrochloride(SKF525 A) was added into the blood samples(adjusting pH to > 12 by sodium hydroxide solution). Methcathinone was extracted with ethyl acetate. The extract was volatilized with 50 ℃ nitrogen gas flow, and dissolved with methanol and determined by gas chromatography-mass spectrometry. GC-MS conditions: HP-5 MS quartz capillary column(30 m×0.25 mm×0.25 μm); column temperature: the initial temperature was kept at 60 ℃ for 1.5 min, the heating rate was 10 ℃·min~(-1) to 200 ℃ and kept 10 min, and the heating rate was 5 ℃·min~(-1) to 250 ℃ and kept 5 min; the interface temperature was 280 ℃; ion source: EI source, temperature 230 ℃; quadrupole temperature: 150 ℃; scanning mode: SCAN 40-450 amu, SIM methcathinone m/z 58, 77, 105, SKF525 A m/z 86, 99, 165. Results Favorable linearity was obtained at 20-2000 ng·m L~(-1), the linear equation was y = 0.3053×10~(-3) x + 0.0112(r = 0.999), and the detection limit was 10 ng·m L~(-1). At the spike level of 100-1000 ng·m L~(-1), the average relative recovery was at 92.6%-98.9%, the absolute recovery was at 81.6%-86.6% with RSDs at 6.5%-8.9%(n = 5), and the intra-day and inter-day precision were between 7.0%-8.8%. Conclusion This method is simple and sensitive enough to determine methcathinone in the blood.
Objective To develope a forensic method to determine methcathinone in the blood. Methods Proadifen hydrochloride(SKF525 A) was added into the blood samples(adjusting pH to > 12 by sodium hydroxide solution). Methcathinone was extracted with ethyl acetate. The extract was volatilized with 50 ℃ nitrogen gas flow, and dissolved with methanol and determined by gas chromatography-mass spectrometry. GC-MS conditions: HP-5 MS quartz capillary column(30 m×0.25 mm×0.25 μm); column temperature: the initial temperature was kept at 60 ℃ for 1.5 min, the heating rate was 10 ℃·min~(-1) to 200 ℃ and kept 10 min, and the heating rate was 5 ℃·min~(-1) to 250 ℃ and kept 5 min; the interface temperature was 280 ℃; ion source: EI source, temperature 230 ℃; quadrupole temperature: 150 ℃; scanning mode: SCAN 40-450 amu, SIM methcathinone m/z 58, 77, 105, SKF525 A m/z 86, 99, 165. Results Favorable linearity was obtained at 20-2000 ng·m L~(-1), the linear equation was y = 0.3053×10~(-3) x + 0.0112(r = 0.999), and the detection limit was 10 ng·m L~(-1). At the spike level of 100-1000 ng·m L~(-1), the average relative recovery was at 92.6%-98.9%, the absolute recovery was at 81.6%-86.6% with RSDs at 6.5%-8.9%(n = 5), and the intra-day and inter-day precision were between 7.0%-8.8%. Conclusion This method is simple and sensitive enough to determine methcathinone in the blood.
引文
[1]尚世杰,郭灵军.气相色谱-质谱法检测甲卡西酮及意义[J].河南科技大学学报(医学版),2012,30(4):275-276.
[2]常颖,高利生.甲卡西酮概述及分析方法[J].刑事技术,2011,(5):35-38.
[3]张红波,赵璐.甲卡西酮的GC/MS定量分析方法[J].山西医科大学学报,2013,44(12):939-941.
[4]常颖,张春水,高利生.甲卡西酮的气-质联用法分析1例[J].中国法医学杂志,2011,26(6):500-501.
[5]常颖,高利生.卡西酮、甲卡西酮和4-甲基甲卡西酮的LC-MS/MS分析方法的研究[J].刑事技术,2014,(1):29-30.
[6]常颖,张春水,高利生.甲卡西酮的LC-MS/MS定性定量分析方法[J].化学分析计量,2013,22(3):51-53.
[7]常颖,徐鹏,高利生.甲卡西酮的液相色谱法测定[J].化学分析计量,2012,21(1):67-69.
[8]李文海,邵凯,蔺大伟,等.快速溶剂萃取-气相色谱/质谱法分析血液中的甲卡西酮[J].分析测试技术与仪器,2016,22(3):189-192.
[9]刘冬娴,赵明明. GC-MS分析尿液中甲卡西酮[J].法医学杂志,2017,33(5):506-508.
[10]S?rensen LK. Determination of cathinones and related ephedrines in forensic whole-blood samples by liquid-chromatography-electrospray tandem mass spectrometry[J]. J Chromatogra B Analyt Technol Biomed Life Sci,2011,879(11-12):727-736.
[11]Madeleine JS,Diane MB,Anthony PD. Determination of32 cathinone derivatives and other designer drugs in serum by comprehensive LC-QQQ-MS/MS analysis[J]. Anal Bioanal Chem,2013,405(4):1383-1397.
[12]Usui K,Aramaki T,Hashiyada M,et al. Quantitative analysis of 3,4-dimethylmethcathinone in blood and urine by liquid chromatography-tandem mass spectrometry in a fatal case[J]. Leg Med(Tokyo),2014,16(4):222-226.
[13]Zhang L,Wang ZH,Li H,et al. Simultaneous determination of 12 illicit drugs in whole blood and urine by solid phase extraction and UPLC-MS/MS[J]. J Chromatogra B Analyt Technol Biomed Life Sci,2014,955-956:10-19.
[14]王永静,彭怡,赵晓晓,等.大鼠血浆中百草枯浓度的高效液相色谱法测定及毒代动力学研究[J].中南药学,2018,16(7):963-968.
[2]常颖,高利生.甲卡西酮概述及分析方法[J].刑事技术,2011,(5):35-38.
[3]张红波,赵璐.甲卡西酮的GC/MS定量分析方法[J].山西医科大学学报,2013,44(12):939-941.
[4]常颖,张春水,高利生.甲卡西酮的气-质联用法分析1例[J].中国法医学杂志,2011,26(6):500-501.
[5]常颖,高利生.卡西酮、甲卡西酮和4-甲基甲卡西酮的LC-MS/MS分析方法的研究[J].刑事技术,2014,(1):29-30.
[6]常颖,张春水,高利生.甲卡西酮的LC-MS/MS定性定量分析方法[J].化学分析计量,2013,22(3):51-53.
[7]常颖,徐鹏,高利生.甲卡西酮的液相色谱法测定[J].化学分析计量,2012,21(1):67-69.
[8]李文海,邵凯,蔺大伟,等.快速溶剂萃取-气相色谱/质谱法分析血液中的甲卡西酮[J].分析测试技术与仪器,2016,22(3):189-192.
[9]刘冬娴,赵明明. GC-MS分析尿液中甲卡西酮[J].法医学杂志,2017,33(5):506-508.
[10]S?rensen LK. Determination of cathinones and related ephedrines in forensic whole-blood samples by liquid-chromatography-electrospray tandem mass spectrometry[J]. J Chromatogra B Analyt Technol Biomed Life Sci,2011,879(11-12):727-736.
[11]Madeleine JS,Diane MB,Anthony PD. Determination of32 cathinone derivatives and other designer drugs in serum by comprehensive LC-QQQ-MS/MS analysis[J]. Anal Bioanal Chem,2013,405(4):1383-1397.
[12]Usui K,Aramaki T,Hashiyada M,et al. Quantitative analysis of 3,4-dimethylmethcathinone in blood and urine by liquid chromatography-tandem mass spectrometry in a fatal case[J]. Leg Med(Tokyo),2014,16(4):222-226.
[13]Zhang L,Wang ZH,Li H,et al. Simultaneous determination of 12 illicit drugs in whole blood and urine by solid phase extraction and UPLC-MS/MS[J]. J Chromatogra B Analyt Technol Biomed Life Sci,2014,955-956:10-19.
[14]王永静,彭怡,赵晓晓,等.大鼠血浆中百草枯浓度的高效液相色谱法测定及毒代动力学研究[J].中南药学,2018,16(7):963-968.