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李超,徐多麒,王继芬,等. 高效液相色谱-串联质谱法检验毛发中两种合成大麻素[J]. 科学技术与工程, 2019, 19(28): 30-34.
LI Chao,XU Duo-qi,et al.Determination of two synthetic cannabinoids in hair by high performance liquid chromatography-tandem mass spectrometry[J].Science Technology and Engineering,2019,19(28):30-34.
高效液相色谱-串联质谱法检验毛发中两种合成大麻素
Determination of two synthetic cannabinoids in hair by high performance liquid chromatography-tandem mass spectrometry
投稿时间:2019-03-20  修订日期:2019-04-30
DOI:
中文关键词:  合成大麻素  毛发  高效液相色谱-串联质谱  球形研磨酸性甲醇超声提取
英文关键词:synthetic cannabinoid  hair  high performance liquid chromatography-tandem mass spectrometry  ultrasonic extraction of acidic methanol  
基金项目:国家重点研发计划项目(2017YFC0803604-2),证据科学教育部重点实验室开放(2018KFKT01)资助第一
                 
作者单位
李超 中国人民公安大学刑事科学技术学院
徐多麒 中国政法大学
王继芬 中国人民公安大学刑事科学技术学院
覃士扬 北京市公安局司法鉴定中心
辛国斌 北京市公安局司法鉴定中心
王燕燕 北京市公安局司法鉴定中心
摘要点击次数: 233
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中文摘要:
      本文建立了同时分析毛发中AM-2201和JWH-073两种合成大麻素的高效液相色谱-串联质谱方法。分别考察了球形研磨酸性甲醇超声提取、碱消解和酸消解3种毛发的前处理方法,通过回收率和基质效应,总结了3种前处理方法的优缺点。球形研磨甲醇超声提取,将毛发研磨成粉末后,使用酸化后的甲醇超声提取4h,离心,过膜,进样;碱消解,70℃下1mol/L的NaOH溶液水浴30min,乙酸乙酯提取,添加少量NaCl使溶液饱和,振荡,离心,取有机层氮气吹干,甲醇复溶,过膜,进样;酸消解,40℃下0.1%HCl溶液水浴过夜,乙酸乙酯提取,添加少量NaCl使溶液饱和,振荡,离心,取有机层氮气吹干,甲醇复溶,过膜,进样。选用ZORBAX Ecilpse Pluse C18色谱柱,以A相0.1% 甲酸-水(5mmol/L乙酸铵)和B相甲醇作为流动相进行梯度洗脱,电喷雾电离,正离子模式扫描,多反应监测(MRM)模式检测毛发中的AM-2201和JWH-073。AM-2201和JWH-073在0.5~500pg/mg范围内线性关系良好(R2≧0.9997);3个添加水平(5、50、500pg/mg)下,球形研磨酸性甲醇超声提取的回收率在89.4%~94.3%之间,碱消解的回收率在80.9%~94.8%之间,酸消解的回收率在62.3%~78.0%之间;检出限(S/N=3)分别为0.05pg/mg(AM-2201)和0.01pg/mg(JWH-073),定量限(S/N=10)分别为0.1pg/mg(AM-2201)和0.06pg/mg(JWH-073)。
英文摘要:
      A method for the determination of JWH-073 and AM-2201 in liquid hair by liquid chromatography-tandem mass spectrometry was established. The pretreatment methods of ultrasonic extraction, alkali digestion and acid digestion of three kinds of hair were investigated respectively. The advantages and disadvantages of the three pretreatment methods were summarized by the recovery rate and matrix effect. Ultrasonic extraction of methanol, grinding the hair into powder, ultrasonic extraction with methanol for 4h, centrifugation, membrane, injection; alkali digestion, 1mol / L NaOH solution water bath for 30min under 70℃, ethyl acetate extraction, adding a small amount of NaCl to make the solution Saturated, oscillated, centrifuged, taken organic layer nitrogen blow dry, methanol reconstituted, membrane, injection; acid digestion, 0.1% HCl solution water bath overnight under 40℃, ethyl acetate extraction, adding a small amount of NaCl to make the solution saturated, shaking, After centrifugation, the organic layer was blown dry with nitrogen, reconstituted with methanol, passed through the membrane, and injected. ZORBAX Ecilpse Pluse C18 column was used for gradient elution with phase A 0.1% formic acid-water (5 mmol/L ammonium acetate) and phase B methanol as mobile phase. Electrospray ionization, positive ion mode scanning, multiple reaction monitoring (MRM) The pattern detects JWH-073 and AM-2201 in the hair. The linear relationship between JWH-073 and AM-2201 in the range of 0.5~200ng/mL is good (R2≧0.9995). Under the three addition levels (5, 50, 100ng/mL), the recovery of methanol ultrasonic extraction is 89.8%~96.3. Between the %, the recovery of alkali digestion is between 80.9% and 94.8%, the recovery rate of acid digestion is between 62.3% and 78.0%, and the detection limit (S/N=3) is 0.05 ng/mL (JWH). -073) and 0.03 ng/mL (AM-2201), the limit of quantification (S/N = 10) were 0.1 ng/mL (JWH-073) and 0.35 ng/mL (AM-2201).
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