法医学杂志 ›› 2023, Vol. 39 ›› Issue (2): 151-160.DOI: 10.12116/j.issn.1004-5619.2022.321101
收稿日期:
2022-11-07
发布日期:
2023-06-06
出版日期:
2023-04-25
通讯作者:
严慧,沈敏
作者简介:
纪佼佼(1995—),女,博士研究生,主要从事法医毒物分析研究;E-mail:845999211@qq.com
基金资助:
Jiao-jiao JI(), Duo-qi XU, Ping XIANG, Hui YAN(
), Min SHEN(
)
Received:
2022-11-07
Online:
2023-06-06
Published:
2023-04-25
Contact:
Hui YAN, Min SHEN
摘要:
目的 建立一种基于单根头发微分段技术的LC-MS/MS分析方法,并对42种精神活性物质在0.4 mm头发节段中的检测进行验证。 方法 将每根头发剪成0.4 mm长的片段,超声提取,并在含二硫苏糖醇的提取液中浸泡。流动相A为含20 mmol/L乙酸铵、0.1%甲酸、5%乙腈的水溶液,流动相B为乙腈,采用电喷雾离子源正离子模式,在多反应监测模式下采集数据。 结果 单根头发中42种精神活性物质在各自线性范围内线性关系良好(r>0.99),检出限为0.2~10 pg/mm,最低定量限为0.5~20 pg/mm,日内、日间精密度为1.5%~12.7%,日内、日间准确度为86.5%~109.2%,提取回收率为68.1%~98.2%,基质效应为71.3%~111.7%。应用该方法对单次服用唑吡坦28 d的志愿者头发样本进行分析,5根头发中唑吡坦的检出位置位于近根端1.08~1.60 cm,浓度范围为0.62~20.5 pg/mm。 结论 单根毛发微分段分析技术可应用于药物辅助性犯罪案件的调查。
中图分类号:
纪佼佼, 徐多麒, 向平, 严慧, 沈敏. 基于微分段技术分析单根头发中42种精神活性物质[J]. 法医学杂志, 2023, 39(2): 151-160.
Jiao-jiao JI, Duo-qi XU, Ping XIANG, Hui YAN, Min SHEN. Analysis of Forty-Two Psychoactive Substances in a Single Hair by Micro-Segmental Technique[J]. Journal of Forensic Medicine, 2023, 39(2): 151-160.
时间/min | 流速/(mL·min-1) | 流动相A/% | 流动相B/% |
---|---|---|---|
0 | 0.2 | 75 | 25 |
1.0 | 0.2 | 75 | 25 |
8.0 | 0.4 | 50 | 50 |
14.0 | 0.4 | 10 | 90 |
14.5 | 0.4 | 75 | 25 |
16.0 | 0.2 | 75 | 25 |
表1 梯度洗脱程序
Tab. 1 Gradient elution procedure
时间/min | 流速/(mL·min-1) | 流动相A/% | 流动相B/% |
---|---|---|---|
0 | 0.2 | 75 | 25 |
1.0 | 0.2 | 75 | 25 |
8.0 | 0.4 | 50 | 50 |
14.0 | 0.4 | 10 | 90 |
14.5 | 0.4 | 75 | 25 |
16.0 | 0.2 | 75 | 25 |
化合物 | 前体离子(m/z) | 产物离子(m/z) | 去簇电压/V | 碰撞能量/eV | 保留时间/min |
---|---|---|---|---|---|
苯丙胺 | 136.1 | 119.11)/91.1 | 60 | 11/22 | 5.24 |
甲基苯丙胺 | 150.1 | 119.11)/91.1 | 50 | 14/23 | 6.39 |
氯胺酮 | 238.1 | 179.11)/125.1 | 60 | 24/35 | 6.63 |
吗啡 | 286.1 | 201.21)/165.3 | 80 | 35/52 | 2.62 |
O6-单乙酰吗啡 | 328.1 | 211.31)/165.3 | 80 | 36/48 | 4.70 |
可卡因 | 304.1 | 182.21)/150.2 | 60 | 28/35 | 6.56 |
苯甲酰爱康宁 | 290.2 | 168.31)/105.2 | 70 | 26/43 | 1.40 |
麦角二乙胺 | 324.2 | 223.21)/208.2 | 60 | 33/43 | 5.77 |
芬太尼 | 337.2 | 188.31)/104.9 | 20 | 27/13 | 3.76 |
地芬尼多 | 310.0 | 292.61)/129.4 | 60 | 26/40 | 8.03 |
氟硝西泮 | 314.2 | 268.31)/239.3 | 60 | 35/45 | 6.15 |
7-氨基氟硝西泮 | 284.2 | 135.21)/226.2 | 60 | 39/41 | 3.62 |
三唑仑 | 343.2 | 308.21)/315.2 | 60 | 36/35 | 5.46 |
α-羟基三唑仑 | 359.2 | 331.21)/176.1 | 60 | 38/37 | 4.13 |
可待因 | 300.2 | 199.21)/165.3 | 80 | 40/52 | 3.78 |
地西泮 | 285.1 | 193.31)/154.1 | 80 | 45/36 | 6.65 |
去甲地西泮 | 271.2 | 140.21)/208.1 | 70 | 36/36 | 5.44 |
替马西泮 | 301.2 | 255.21)/283.1 | 70 | 36/19 | 5.52 |
奥沙西泮 | 287.2 | 241.21)/269.3 | 50 | 31/21 | 4.42 |
阿普唑仑 | 309.1 | 281.11)/274.2 | 60 | 33/32 | 5.46 |
α-羟基阿普唑仑 | 325.2 | 297.21)/279.2 | 70 | 35/33 | 4.17 |
氯硝西泮 | 316.2 | 270.11)/214.1 | 60 | 36/49 | 5.36 |
7-氨基氯硝西泮 | 286.1 | 222.21)/250.1 | 40 | 34/25 | 2.92 |
艾司唑仑 | 295.2 | 267.31)/205.2 | 50 | 34/53 | 4.84 |
劳拉西泮 | 321.1 | 275.11)/303.1 | 50 | 30/21 | 4.60 |
咪达唑仑 | 326.2 | 291.41)/244.2 | 50 | 37/37 | 9.39 |
硝西泮 | 282.2 | 236.21)/180.2 | 50 | 35/32 | 5.05 |
7-氨基硝西泮 | 252.1 | 121.11)/146.2 | 60 | 52/37 | 2.90 |
唑吡坦 | 308.1 | 235.11)/263.2 | 40 | 38/53 | 9.29 |
西酞普兰 | 325.3 | 109.21)/262.0 | 60 | 35/41 | 13.32 |
苯海拉明 | 256.2 | 167.21)/165.2 | 30 | 26/17 | 13.64 |
右美沙芬 | 272.3 | 147.21)/213.3 | 60 | 54/42 | 12.31 |
氯氮平 | 327.3 | 270.11)/296.3 | 70 | 28/32 | 10.90 |
东莨菪碱 | 304.3 | 138.31)/156.3 | 60 | 33/31 | 4.34 |
右美托咪定 | 201.1 | 68.11)/94.8 | 60 | 23/40 | 9.39 |
曲马多 | 264.2 | 58.01)/246.2 | 50 | 24/37 | 8.46 |
安替比林 | 189.0 | 56.01)/77.0 | 60 | 16/27 | 2.59 |
卡马西平 | 237.3 | 194.31)/192.3 | 60 | 37/26 | 4.16 |
奥卡西平 | 253.0 | 235.91)/208.1 | 70 | 32/19 | 3.47 |
尼美西泮 | 296.1 | 250.21)/222.1 | 70 | 20/36 | 6.13 |
喹硫平 | 384.4 | 253.11)/221.0 | 54 | 30/35 | 10.10 |
米氮平 | 266.1 | 195.11)/208.8 | 80 | 37/35 | 7.81 |
氯胺酮-d4 | 242.2 | 183.11)/129.2 | 60 | 26/40 | 6.81 |
地西泮-d5 | 290.2 | 198.21)/154.4 | 60 | 46/40 | 6.50 |
喹硫平-d8 | 392.2 | 258.11)/226.1 | 40 | 31/50 | 10.30 |
表2 42种精神活性物质及3种内标的MRM参数和保留时间
Tab. 2 MRM parameters and retention times for 42 psychoactive substances and 3 internal standard substances
化合物 | 前体离子(m/z) | 产物离子(m/z) | 去簇电压/V | 碰撞能量/eV | 保留时间/min |
---|---|---|---|---|---|
苯丙胺 | 136.1 | 119.11)/91.1 | 60 | 11/22 | 5.24 |
甲基苯丙胺 | 150.1 | 119.11)/91.1 | 50 | 14/23 | 6.39 |
氯胺酮 | 238.1 | 179.11)/125.1 | 60 | 24/35 | 6.63 |
吗啡 | 286.1 | 201.21)/165.3 | 80 | 35/52 | 2.62 |
O6-单乙酰吗啡 | 328.1 | 211.31)/165.3 | 80 | 36/48 | 4.70 |
可卡因 | 304.1 | 182.21)/150.2 | 60 | 28/35 | 6.56 |
苯甲酰爱康宁 | 290.2 | 168.31)/105.2 | 70 | 26/43 | 1.40 |
麦角二乙胺 | 324.2 | 223.21)/208.2 | 60 | 33/43 | 5.77 |
芬太尼 | 337.2 | 188.31)/104.9 | 20 | 27/13 | 3.76 |
地芬尼多 | 310.0 | 292.61)/129.4 | 60 | 26/40 | 8.03 |
氟硝西泮 | 314.2 | 268.31)/239.3 | 60 | 35/45 | 6.15 |
7-氨基氟硝西泮 | 284.2 | 135.21)/226.2 | 60 | 39/41 | 3.62 |
三唑仑 | 343.2 | 308.21)/315.2 | 60 | 36/35 | 5.46 |
α-羟基三唑仑 | 359.2 | 331.21)/176.1 | 60 | 38/37 | 4.13 |
可待因 | 300.2 | 199.21)/165.3 | 80 | 40/52 | 3.78 |
地西泮 | 285.1 | 193.31)/154.1 | 80 | 45/36 | 6.65 |
去甲地西泮 | 271.2 | 140.21)/208.1 | 70 | 36/36 | 5.44 |
替马西泮 | 301.2 | 255.21)/283.1 | 70 | 36/19 | 5.52 |
奥沙西泮 | 287.2 | 241.21)/269.3 | 50 | 31/21 | 4.42 |
阿普唑仑 | 309.1 | 281.11)/274.2 | 60 | 33/32 | 5.46 |
α-羟基阿普唑仑 | 325.2 | 297.21)/279.2 | 70 | 35/33 | 4.17 |
氯硝西泮 | 316.2 | 270.11)/214.1 | 60 | 36/49 | 5.36 |
7-氨基氯硝西泮 | 286.1 | 222.21)/250.1 | 40 | 34/25 | 2.92 |
艾司唑仑 | 295.2 | 267.31)/205.2 | 50 | 34/53 | 4.84 |
劳拉西泮 | 321.1 | 275.11)/303.1 | 50 | 30/21 | 4.60 |
咪达唑仑 | 326.2 | 291.41)/244.2 | 50 | 37/37 | 9.39 |
硝西泮 | 282.2 | 236.21)/180.2 | 50 | 35/32 | 5.05 |
7-氨基硝西泮 | 252.1 | 121.11)/146.2 | 60 | 52/37 | 2.90 |
唑吡坦 | 308.1 | 235.11)/263.2 | 40 | 38/53 | 9.29 |
西酞普兰 | 325.3 | 109.21)/262.0 | 60 | 35/41 | 13.32 |
苯海拉明 | 256.2 | 167.21)/165.2 | 30 | 26/17 | 13.64 |
右美沙芬 | 272.3 | 147.21)/213.3 | 60 | 54/42 | 12.31 |
氯氮平 | 327.3 | 270.11)/296.3 | 70 | 28/32 | 10.90 |
东莨菪碱 | 304.3 | 138.31)/156.3 | 60 | 33/31 | 4.34 |
右美托咪定 | 201.1 | 68.11)/94.8 | 60 | 23/40 | 9.39 |
曲马多 | 264.2 | 58.01)/246.2 | 50 | 24/37 | 8.46 |
安替比林 | 189.0 | 56.01)/77.0 | 60 | 16/27 | 2.59 |
卡马西平 | 237.3 | 194.31)/192.3 | 60 | 37/26 | 4.16 |
奥卡西平 | 253.0 | 235.91)/208.1 | 70 | 32/19 | 3.47 |
尼美西泮 | 296.1 | 250.21)/222.1 | 70 | 20/36 | 6.13 |
喹硫平 | 384.4 | 253.11)/221.0 | 54 | 30/35 | 10.10 |
米氮平 | 266.1 | 195.11)/208.8 | 80 | 37/35 | 7.81 |
氯胺酮-d4 | 242.2 | 183.11)/129.2 | 60 | 26/40 | 6.81 |
地西泮-d5 | 290.2 | 198.21)/154.4 | 60 | 46/40 | 6.50 |
喹硫平-d8 | 392.2 | 258.11)/226.1 | 40 | 31/50 | 10.30 |
图1 空白头发(A)与空白头发添加20 pg/mm 42种精神活性物质(B)的色谱图
Fig. 1 The chromatograms of hair collecting before administration (A) and 42 psychoactive substances spiked at 20 pg/mm (B)
化合物 | 线性范围/ (pg·mm-1) | 回归方程 | 相关系数(r) | LOD/ (pg·mm-1) | LLOQ/ (pg·mm-1) | 内标 |
---|---|---|---|---|---|---|
苯丙胺 | 5~500 | y=0.207 83 x+3.045 54 | 0.993 96 | 2 | 5 | 氯胺酮-d4 |
甲基苯丙胺 | 20~500 | y=0.744 31 x+4.803 91 | 0.994 28 | 5 | 20 | 氯胺酮-d4 |
氯胺酮 | 10~500 | y=1.216 12 x+2.136 96 | 0.997 66 | 2 | 10 | 氯胺酮-d4 |
吗啡 | 20~500 | y=0.021 54 x+0.660 82 | 0.993 31 | 10 | 20 | 氯胺酮-d4 |
甲基苯丙胺 | 20~500 | y=0.744 31 x+4.803 91 | 0.994 28 | 5 | 20 | 氯胺酮-d4 |
氯胺酮 | 10~500 | y=1.216 12 x+2.136 96 | 0.997 66 | 2 | 10 | 氯胺酮-d4 |
O6-单乙酰吗啡 | 20~500 | y=0.004 43 x+0.546 90 | 0.993 02 | 5 | 20 | 氯胺酮-d4 |
可卡因 | 5~500 | y=1.951 38 x+3.168 50 | 0.994 17 | 2 | 5 | 氯胺酮-d4 |
苯甲酰爱康宁 | 2~500 | y=2.720 58 x+0.919 45 | 0.997 93 | 1 | 2 | 氯胺酮-d4 |
麦角二乙胺 | 1~500 | y=2.354 68 x+0.426 31 | 0.997 55 | 0.5 | 1 | 氯胺酮-d4 |
芬太尼 | 20~500 | y=1.152 65 x-9.790 53 | 0.990 28 | 10 | 20 | 氯胺酮-d4 |
地芬尼多 | 10~500 | y=1.332 11 x+2.886 06 | 0.993 25 | 2 | 10 | 喹硫平-d8 |
氟硝西泮 | 2~500 | y=0.042 87 x-0.063 26 | 0.995 18 | 0.5 | 2 | 地西泮-d5 |
7-氨基氟硝西泮 | 2~500 | y=0.072 76 x-0.146 79 | 0.996 68 | 0.5 | 2 | 地西泮-d5 |
三唑仑 | 1~500 | y=0.055 27 x-0.031 23 | 0.994 24 | 0.2 | 1 | 地西泮-d5 |
α-羟基三唑仑 | 5~500 | y=0.008 25 x+0.003 83 | 0.994 26 | 1 | 5 | 地西泮-d5 |
可待因 | 20~500 | y=0.057 99 x+1.219 88 | 0.998 88 | 5 | 20 | 地西泮-d5 |
地西泮 | 1~500 | y=0.310 37 x+1.076 27 | 0.995 08 | 0.2 | 1 | 地西泮-d5 |
去甲地西泮 | 5~500 | y=0.117 61 x+2.319 53 | 0.994 32 | 1 | 5 | 地西泮-d5 |
替马西泮 | 10~500 | y=0.543 24 x+1.570 80 | 0.995 76 | 5 | 10 | 地西泮-d5 |
奥沙西泮 | 20~500 | y=0.077 60 x+6.031 51 | 0.997 49 | 10 | 20 | 地西泮-d5 |
阿普唑仑 | 2~500 | y=0.505 37 x+1.623 54 | 0.995 75 | 0.5 | 2 | 地西泮-d5 |
α-羟基阿普唑仑 | 10~500 | y=0.128 46 x+0.991 37 | 0.991 39 | 2 | 10 | 地西泮-d5 |
氯硝西泮 | 5~500 | y=0.196 84 x+1.842 02 | 0.995 11 | 1 | 5 | 地西泮-d5 |
7-氨基氯硝西泮 | 2~500 | y=0.160 57 x+1.340 30 | 0.993 32 | 1 | 2 | 地西泮-d5 |
艾司唑仑 | 1~500 | y=1.336 01 x+0.224 92 | 0.998 56 | 0.2 | 1 | 地西泮-d5 |
劳拉西泮 | 20~500 | y=0.049 56 x+0.462 25 | 0.996 62 | 10 | 20 | 地西泮-d5 |
咪达唑仑 | 1~500 | y=2.790 51 x+0.312 17 | 0.997 59 | 0.5 | 1 | 地西泮-d5 |
硝西泮 | 5~500 | y=0.234 00 x+1.193 09 | 0.994 09 | 2 | 5 | 地西泮-d5 |
7-氨基硝西泮 | 10~500 | y=0.542 20 x+8.245 20 | 0.993 77 | 5 | 10 | 地西泮-d5 |
唑吡坦 | 0.5~500 | y=6.173 96 x+0.222 13 | 0.995 16 | 0.1 | 0.5 | 地西泮-d5 |
西酞普兰 | 2~500 | y=7.322 17 x+1.558 15 | 0.998 04 | 0.5 | 2 | 喹硫平-d8 |
苯海拉明 | 2~500 | y=0.785 10 x+1.299 34 | 0.997 54 | 1 | 2 | 喹硫平-d8 |
右美沙芬 | 10~500 | y=0.243 66 x+7.096 43 | 0.993 61 | 2 | 10 | 喹硫平-d8 |
氯氮平 | 2~500 | y=2.494 10 x+6.650 52 | 0.993 80 | 1 | 2 | 喹硫平-d8 |
东莨菪碱 | 0.5~500 | y=1.567 98 x-0.120 40 | 0.996 04 | 0.2 | 0.5 | 喹硫平-d8 |
右美托咪定 | 5~500 | y=0.333 05 x+2.030 27 | 0.994 15 | 2 | 5 | 喹硫平-d8 |
曲马多 | 20~500 | y=0.557 97 x+7.067 36 | 0.996 66 | 10 | 20 | 喹硫平-d8 |
安替比林 | 20~500 | y=0.019 51 x+2.472 81 | 0.994 99 | 5 | 20 | 喹硫平-d8 |
卡马西平 | 5~500 | y=2.121 50 x+1.417 83 | 0.997 63 | 2 | 5 | 喹硫平-d8 |
奥卡西平 | 10~500 | y=0.335 85 x+6.422 52 | 0.994 89 | 5 | 10 | 喹硫平-d8 |
尼美西泮 | 2~500 | y=0.519 45 x+0.488 19 | 0.995 54 | 1 | 2 | 地西泮-d5 |
喹硫平 | 2~500 | y=6.655 51 x+1.312 71 | 0.994 33 | 1 | 2 | 喹硫平-d8 |
米氮平 | 0.5~500 | y=4.556 82 x+0.015 92 | 0.996 80 | 0.2 | 0.5 | 喹硫平-d8 |
表3 头发中42种精神活性物质的回归方程、相关系数(r)、LOD和LLOQ
Tab. 3 Regression equation, correlation coefficient ( r ), LOD and LLOQ of 42 psychoactive substances in hair
化合物 | 线性范围/ (pg·mm-1) | 回归方程 | 相关系数(r) | LOD/ (pg·mm-1) | LLOQ/ (pg·mm-1) | 内标 |
---|---|---|---|---|---|---|
苯丙胺 | 5~500 | y=0.207 83 x+3.045 54 | 0.993 96 | 2 | 5 | 氯胺酮-d4 |
甲基苯丙胺 | 20~500 | y=0.744 31 x+4.803 91 | 0.994 28 | 5 | 20 | 氯胺酮-d4 |
氯胺酮 | 10~500 | y=1.216 12 x+2.136 96 | 0.997 66 | 2 | 10 | 氯胺酮-d4 |
吗啡 | 20~500 | y=0.021 54 x+0.660 82 | 0.993 31 | 10 | 20 | 氯胺酮-d4 |
甲基苯丙胺 | 20~500 | y=0.744 31 x+4.803 91 | 0.994 28 | 5 | 20 | 氯胺酮-d4 |
氯胺酮 | 10~500 | y=1.216 12 x+2.136 96 | 0.997 66 | 2 | 10 | 氯胺酮-d4 |
O6-单乙酰吗啡 | 20~500 | y=0.004 43 x+0.546 90 | 0.993 02 | 5 | 20 | 氯胺酮-d4 |
可卡因 | 5~500 | y=1.951 38 x+3.168 50 | 0.994 17 | 2 | 5 | 氯胺酮-d4 |
苯甲酰爱康宁 | 2~500 | y=2.720 58 x+0.919 45 | 0.997 93 | 1 | 2 | 氯胺酮-d4 |
麦角二乙胺 | 1~500 | y=2.354 68 x+0.426 31 | 0.997 55 | 0.5 | 1 | 氯胺酮-d4 |
芬太尼 | 20~500 | y=1.152 65 x-9.790 53 | 0.990 28 | 10 | 20 | 氯胺酮-d4 |
地芬尼多 | 10~500 | y=1.332 11 x+2.886 06 | 0.993 25 | 2 | 10 | 喹硫平-d8 |
氟硝西泮 | 2~500 | y=0.042 87 x-0.063 26 | 0.995 18 | 0.5 | 2 | 地西泮-d5 |
7-氨基氟硝西泮 | 2~500 | y=0.072 76 x-0.146 79 | 0.996 68 | 0.5 | 2 | 地西泮-d5 |
三唑仑 | 1~500 | y=0.055 27 x-0.031 23 | 0.994 24 | 0.2 | 1 | 地西泮-d5 |
α-羟基三唑仑 | 5~500 | y=0.008 25 x+0.003 83 | 0.994 26 | 1 | 5 | 地西泮-d5 |
可待因 | 20~500 | y=0.057 99 x+1.219 88 | 0.998 88 | 5 | 20 | 地西泮-d5 |
地西泮 | 1~500 | y=0.310 37 x+1.076 27 | 0.995 08 | 0.2 | 1 | 地西泮-d5 |
去甲地西泮 | 5~500 | y=0.117 61 x+2.319 53 | 0.994 32 | 1 | 5 | 地西泮-d5 |
替马西泮 | 10~500 | y=0.543 24 x+1.570 80 | 0.995 76 | 5 | 10 | 地西泮-d5 |
奥沙西泮 | 20~500 | y=0.077 60 x+6.031 51 | 0.997 49 | 10 | 20 | 地西泮-d5 |
阿普唑仑 | 2~500 | y=0.505 37 x+1.623 54 | 0.995 75 | 0.5 | 2 | 地西泮-d5 |
α-羟基阿普唑仑 | 10~500 | y=0.128 46 x+0.991 37 | 0.991 39 | 2 | 10 | 地西泮-d5 |
氯硝西泮 | 5~500 | y=0.196 84 x+1.842 02 | 0.995 11 | 1 | 5 | 地西泮-d5 |
7-氨基氯硝西泮 | 2~500 | y=0.160 57 x+1.340 30 | 0.993 32 | 1 | 2 | 地西泮-d5 |
艾司唑仑 | 1~500 | y=1.336 01 x+0.224 92 | 0.998 56 | 0.2 | 1 | 地西泮-d5 |
劳拉西泮 | 20~500 | y=0.049 56 x+0.462 25 | 0.996 62 | 10 | 20 | 地西泮-d5 |
咪达唑仑 | 1~500 | y=2.790 51 x+0.312 17 | 0.997 59 | 0.5 | 1 | 地西泮-d5 |
硝西泮 | 5~500 | y=0.234 00 x+1.193 09 | 0.994 09 | 2 | 5 | 地西泮-d5 |
7-氨基硝西泮 | 10~500 | y=0.542 20 x+8.245 20 | 0.993 77 | 5 | 10 | 地西泮-d5 |
唑吡坦 | 0.5~500 | y=6.173 96 x+0.222 13 | 0.995 16 | 0.1 | 0.5 | 地西泮-d5 |
西酞普兰 | 2~500 | y=7.322 17 x+1.558 15 | 0.998 04 | 0.5 | 2 | 喹硫平-d8 |
苯海拉明 | 2~500 | y=0.785 10 x+1.299 34 | 0.997 54 | 1 | 2 | 喹硫平-d8 |
右美沙芬 | 10~500 | y=0.243 66 x+7.096 43 | 0.993 61 | 2 | 10 | 喹硫平-d8 |
氯氮平 | 2~500 | y=2.494 10 x+6.650 52 | 0.993 80 | 1 | 2 | 喹硫平-d8 |
东莨菪碱 | 0.5~500 | y=1.567 98 x-0.120 40 | 0.996 04 | 0.2 | 0.5 | 喹硫平-d8 |
右美托咪定 | 5~500 | y=0.333 05 x+2.030 27 | 0.994 15 | 2 | 5 | 喹硫平-d8 |
曲马多 | 20~500 | y=0.557 97 x+7.067 36 | 0.996 66 | 10 | 20 | 喹硫平-d8 |
安替比林 | 20~500 | y=0.019 51 x+2.472 81 | 0.994 99 | 5 | 20 | 喹硫平-d8 |
卡马西平 | 5~500 | y=2.121 50 x+1.417 83 | 0.997 63 | 2 | 5 | 喹硫平-d8 |
奥卡西平 | 10~500 | y=0.335 85 x+6.422 52 | 0.994 89 | 5 | 10 | 喹硫平-d8 |
尼美西泮 | 2~500 | y=0.519 45 x+0.488 19 | 0.995 54 | 1 | 2 | 地西泮-d5 |
喹硫平 | 2~500 | y=6.655 51 x+1.312 71 | 0.994 33 | 1 | 2 | 喹硫平-d8 |
米氮平 | 0.5~500 | y=4.556 82 x+0.015 92 | 0.996 80 | 0.2 | 0.5 | 喹硫平-d8 |
化合物 | 浓度/(pg·mm-1) | 日内(n=6) | 日间(n=24) | 基质效应 (n=6) | 提取回收率 (n=6) | ||
---|---|---|---|---|---|---|---|
精密度 | 准确度 | 精密度 | 准确度 | ||||
苯丙胺 | 5 | 5.7 | 92.5 | 6.2 | 94.8 | 90.1 | 88.2 |
250 | 6.7 | 92.0 | 8.1 | 94.3 | 89.0 | 87.6 | |
甲基苯丙胺 | 20 | 7.8 | 97.5 | 12.6 | 91.3 | 85.0 | 92.5 |
250 | 4.7 | 90.9 | 12.2 | 94.1 | 93.8 | 85.3 | |
氯胺酮 | 10 | 2.9 | 92.7 | 8.1 | 91.6 | 80.4 | 90.7 |
250 | 3.0 | 91.7 | 6.5 | 95.1 | 86.3 | 84.5 | |
吗啡 | 20 | 9.8 | 87.7 | 9.4 | 91.6 | 88.1 | 76.3 |
250 | 2.3 | 91.0 | 5.4 | 92.6 | 89.2 | 83.2 | |
O6-单乙酰吗啡 | 20 | 3.4 | 92.3 | 5.9 | 104.2 | 91.5 | 83.6 |
250 | 3.9 | 93.5 | 8.4 | 92.2 | 87.6 | 77.2 | |
可卡因 | 5 | 4.9 | 94.5 | 7.6 | 99.2 | 90.2 | 84.1 |
250 | 3.9 | 97.2 | 6.1 | 105.3 | 92.4 | 79.2 | |
苯甲酰爱康宁 | 2 | 4.0 | 93.4 | 5.3 | 94.8 | 93.4 | 91.2 |
250 | 2.9 | 99.5 | 4.2 | 98.0 | 94.5 | 90.8 | |
麦角二乙胺 | 1 | 6.1 | 102.1 | 8.8 | 105.2 | 87.2 | 80.5 |
250 | 4.9 | 96.7 | 6.4 | 102.2 | 86.4 | 76.5 | |
芬太尼 | 20 | 5.2 | 92.0 | 9.4 | 89.5 | 71.3 | 79.2 |
250 | 7.9 | 90.5 | 11.2 | 94.5 | 85.4 | 76.2 | |
地芬尼多 | 10 | 5.0 | 95.1 | 3.1 | 92.1 | 89.4 | 85.4 |
250 | 4.1 | 94.3 | 9.4 | 91.5 | 80.6 | 76.2 | |
氟硝西泮 | 2 | 2.4 | 101.9 | 5.3 | 109.2 | 95.4 | 90.6 |
250 | 5.1 | 97.6 | 6.9 | 96.1 | 95.6 | 91.2 | |
7-氨基氟硝西泮 | 2 | 3.9 | 97.1 | 10.5 | 94.7 | 94.5 | 90.6 |
250 | 4.5 | 93.6 | 5.8 | 97.5 | 98.2 | 92.4 | |
三唑仑 | 1 | 3.9 | 102.9 | 8.2 | 109.1 | 86.3 | 88.6 |
250 | 8.4 | 101.3 | 10.8 | 106.8 | 94.3 | 91.5 | |
α-羟基三唑仑 | 5 | 7.1 | 96.1 | 11.2 | 93.9 | 88.5 | 76.2 |
250 | 6.9 | 97.4 | 10.6 | 95.1 | 85.1 | 78.5 | |
可待因 | 20 | 7.9 | 94.9 | 7.9 | 88.2 | 81.2 | 73.5 |
250 | 10.2 | 98.4 | 4.9 | 99.2 | 84.9 | 80.2 | |
地西泮 | 1 | 8.1 | 98.3 | 11.5 | 100.5 | 89.5 | 88.2 |
250 | 6.1 | 102.6 | 8.3 | 104.9 | 92.1 | 91.3 | |
去甲地西泮 | 5 | 4.2 | 98.3 | 9.2 | 95.1 | 90.1 | 74.2 |
250 | 5.7 | 92.3 | 8.0 | 106.0 | 85.9 | 89.6 | |
替马西泮 | 10 | 3.8 | 97.4 | 5.2 | 98.1 | 97.2 | 86.1 |
250 | 2.4 | 92.1 | 4.5 | 104.5 | 94.1 | 88.8 | |
奥沙西泮 | 20 | 5.1 | 103.5 | 12.7 | 103.6 | 94.5 | 91.6 |
250 | 11.8 | 96.8 | 10.2 | 90.4 | 95.6 | 84.5 | |
阿普唑仑 | 2 | 5.1 | 98.1 | 7.7 | 96.6 | 88.5 | 76.9 |
250 | 4.0 | 97.0 | 6.5 | 98.6 | 84.6 | 77.9 | |
α-羟基阿普唑仑 | 10 | 8.2 | 95.0 | 11.6 | 90.5 | 85.9 | 88.6 |
250 | 6.9 | 93.1 | 10.5 | 94.2 | 89.2 | 79.9 | |
氯硝西泮 | 5 | 3.2 | 97.2 | 6.8 | 96.6 | 94.5 | 90.6 |
250 | 4.0 | 96.1 | 5.5 | 93.7 | 92.1 | 89.7 | |
7-氨基氯硝西泮 | 2 | 4.9 | 93.5 | 5.6 | 96.2 | 94.2 | 94.9 |
250 | 5.1 | 94.6 | 9.1 | 96.8 | 96.2 | 89.8 | |
艾司唑仑 | 1 | 1.5 | 95.1 | 5.3 | 98.6 | 102.4 | 92.5 |
250 | 3.9 | 94.2 | 5.6 | 100.9 | 100.8 | 91.8 | |
劳拉西泮 | 20 | 2.1 | 88.4 | 5.6 | 104.6 | 105.2 | 98.2 |
250 | 5.1 | 90.6 | 9.4 | 106.6 | 101.5 | 91.5 | |
咪达唑仑 | 1 | 4.9 | 97.3 | 7.1 | 94.8 | 98.2 | 92.5 |
250 | 2.7 | 100.9 | 8.5 | 97.7 | 103.5 | 86.9 | |
硝西泮 | 5 | 4.8 | 97.5 | 9.4 | 93.2 | 109.3 | 89.9 |
250 | 5.1 | 90.1 | 8.1 | 103.2 | 107.6 | 84.5 | |
7-氨基硝西泮 | 10 | 4.1 | 105.7 | 9.4 | 98.5 | 99.6 | 88.8 |
250 | 2.9 | 94.5 | 6.9 | 91.4 | 97.2 | 76.0 | |
唑吡坦 | 0.5 | 4.2 | 99.2 | 6.7 | 95.4 | 102.1 | 89.0 |
250 | 2.9 | 100.6 | 5.4 | 99.3 | 97.8 | 84.9 | |
西酞普兰 | 2 | 4.9 | 98.5 | 5.9 | 105.3 | 94.2 | 86.9 |
250 | 7.3 | 96.3 | 8.4 | 96.2 | 98.7 | 83.1 | |
苯海拉明 | 2 | 4.5 | 102.4 | 6.3 | 108.6 | 89.4 | 81.1 |
250 | 5.2 | 94.2 | 6.9 | 102.1 | 94.2 | 76.2 | |
右美沙芬 | 10 | 3.6 | 97.5 | 7.5 | 98.0 | 86.5 | 81.9 |
250 | 5.1 | 93.2 | 8.4 | 106.7 | 87.2 | 77.8 | |
氯氮平 | 2 | 1.9 | 98.2 | 6.0 | 99.4 | 91.6 | 87.2 |
250 | 4.2 | 97.2 | 5.5 | 93.8 | 94.2 | 81.7 | |
东莨菪碱 | 0.5 | 2.9 | 86.7 | 5.4 | 92.1 | 89.4 | 86.2 |
250 | 8.4 | 104.9 | 10.5 | 106.0 | 102.8 | 82.4 | |
右美托咪定 | 5 | 4.6 | 98.1 | 11.2 | 97.2 | 91.5 | 71.5 |
250 | 3.5 | 96.2 | 5.6 | 93.4 | 87.5 | 79.1 | |
曲马多 | 20 | 9.4 | 91.5 | 6.9 | 105.2 | 94.2 | 68.1 |
250 | 2.7 | 94.5 | 3.9 | 93.6 | 88.5 | 71.1 | |
安替比林 | 20 | 4.9 | 86.5 | 7.5 | 103.6 | 105.4 | 84.3 |
250 | 1.8 | 90.5 | 2.8 | 94.5 | 94.1 | 88.4 | |
卡马西平 | 5 | 2.1 | 98.4 | 5.7 | 97.9 | 102.7 | 75.4 |
250 | 3.8 | 98.2 | 7.8 | 96.3 | 97.5 | 82.6 | |
奥卡西平 | 10 | 3.6 | 97.1 | 9.3 | 96.5 | 100.2 | 89.4 |
250 | 4.2 | 102.9 | 6.5 | 100.1 | 104.6 | 79.2 | |
尼美西泮 | 2 | 5.1 | 98.2 | 8.8 | 96.8 | 88.9 | 87.2 |
250 | 4.6 | 101.7 | 6.7 | 105.5 | 89.4 | 84.9 | |
喹硫平 | 2 | 1.7 | 98.2 | 6.0 | 101.8 | 102.7 | 94.2 |
250 | 2.0 | 97.2 | 7.4 | 101.7 | 103.8 | 90.8 | |
米氮平 | 0.5 | 1.9 | 98.3 | 3.1 | 97.2 | 111.7 | 86.4 |
250 | 2.3 | 103.2 | 9.7 | 103.5 | 102.7 | 91.6 |
表4 头发中42种精神活性物质的精密度、准确度、回收率和基质效应 (%)
Tab. 4 Precision, accuracy, recovery and matrix effect of 42 psychoactive substances in hair
化合物 | 浓度/(pg·mm-1) | 日内(n=6) | 日间(n=24) | 基质效应 (n=6) | 提取回收率 (n=6) | ||
---|---|---|---|---|---|---|---|
精密度 | 准确度 | 精密度 | 准确度 | ||||
苯丙胺 | 5 | 5.7 | 92.5 | 6.2 | 94.8 | 90.1 | 88.2 |
250 | 6.7 | 92.0 | 8.1 | 94.3 | 89.0 | 87.6 | |
甲基苯丙胺 | 20 | 7.8 | 97.5 | 12.6 | 91.3 | 85.0 | 92.5 |
250 | 4.7 | 90.9 | 12.2 | 94.1 | 93.8 | 85.3 | |
氯胺酮 | 10 | 2.9 | 92.7 | 8.1 | 91.6 | 80.4 | 90.7 |
250 | 3.0 | 91.7 | 6.5 | 95.1 | 86.3 | 84.5 | |
吗啡 | 20 | 9.8 | 87.7 | 9.4 | 91.6 | 88.1 | 76.3 |
250 | 2.3 | 91.0 | 5.4 | 92.6 | 89.2 | 83.2 | |
O6-单乙酰吗啡 | 20 | 3.4 | 92.3 | 5.9 | 104.2 | 91.5 | 83.6 |
250 | 3.9 | 93.5 | 8.4 | 92.2 | 87.6 | 77.2 | |
可卡因 | 5 | 4.9 | 94.5 | 7.6 | 99.2 | 90.2 | 84.1 |
250 | 3.9 | 97.2 | 6.1 | 105.3 | 92.4 | 79.2 | |
苯甲酰爱康宁 | 2 | 4.0 | 93.4 | 5.3 | 94.8 | 93.4 | 91.2 |
250 | 2.9 | 99.5 | 4.2 | 98.0 | 94.5 | 90.8 | |
麦角二乙胺 | 1 | 6.1 | 102.1 | 8.8 | 105.2 | 87.2 | 80.5 |
250 | 4.9 | 96.7 | 6.4 | 102.2 | 86.4 | 76.5 | |
芬太尼 | 20 | 5.2 | 92.0 | 9.4 | 89.5 | 71.3 | 79.2 |
250 | 7.9 | 90.5 | 11.2 | 94.5 | 85.4 | 76.2 | |
地芬尼多 | 10 | 5.0 | 95.1 | 3.1 | 92.1 | 89.4 | 85.4 |
250 | 4.1 | 94.3 | 9.4 | 91.5 | 80.6 | 76.2 | |
氟硝西泮 | 2 | 2.4 | 101.9 | 5.3 | 109.2 | 95.4 | 90.6 |
250 | 5.1 | 97.6 | 6.9 | 96.1 | 95.6 | 91.2 | |
7-氨基氟硝西泮 | 2 | 3.9 | 97.1 | 10.5 | 94.7 | 94.5 | 90.6 |
250 | 4.5 | 93.6 | 5.8 | 97.5 | 98.2 | 92.4 | |
三唑仑 | 1 | 3.9 | 102.9 | 8.2 | 109.1 | 86.3 | 88.6 |
250 | 8.4 | 101.3 | 10.8 | 106.8 | 94.3 | 91.5 | |
α-羟基三唑仑 | 5 | 7.1 | 96.1 | 11.2 | 93.9 | 88.5 | 76.2 |
250 | 6.9 | 97.4 | 10.6 | 95.1 | 85.1 | 78.5 | |
可待因 | 20 | 7.9 | 94.9 | 7.9 | 88.2 | 81.2 | 73.5 |
250 | 10.2 | 98.4 | 4.9 | 99.2 | 84.9 | 80.2 | |
地西泮 | 1 | 8.1 | 98.3 | 11.5 | 100.5 | 89.5 | 88.2 |
250 | 6.1 | 102.6 | 8.3 | 104.9 | 92.1 | 91.3 | |
去甲地西泮 | 5 | 4.2 | 98.3 | 9.2 | 95.1 | 90.1 | 74.2 |
250 | 5.7 | 92.3 | 8.0 | 106.0 | 85.9 | 89.6 | |
替马西泮 | 10 | 3.8 | 97.4 | 5.2 | 98.1 | 97.2 | 86.1 |
250 | 2.4 | 92.1 | 4.5 | 104.5 | 94.1 | 88.8 | |
奥沙西泮 | 20 | 5.1 | 103.5 | 12.7 | 103.6 | 94.5 | 91.6 |
250 | 11.8 | 96.8 | 10.2 | 90.4 | 95.6 | 84.5 | |
阿普唑仑 | 2 | 5.1 | 98.1 | 7.7 | 96.6 | 88.5 | 76.9 |
250 | 4.0 | 97.0 | 6.5 | 98.6 | 84.6 | 77.9 | |
α-羟基阿普唑仑 | 10 | 8.2 | 95.0 | 11.6 | 90.5 | 85.9 | 88.6 |
250 | 6.9 | 93.1 | 10.5 | 94.2 | 89.2 | 79.9 | |
氯硝西泮 | 5 | 3.2 | 97.2 | 6.8 | 96.6 | 94.5 | 90.6 |
250 | 4.0 | 96.1 | 5.5 | 93.7 | 92.1 | 89.7 | |
7-氨基氯硝西泮 | 2 | 4.9 | 93.5 | 5.6 | 96.2 | 94.2 | 94.9 |
250 | 5.1 | 94.6 | 9.1 | 96.8 | 96.2 | 89.8 | |
艾司唑仑 | 1 | 1.5 | 95.1 | 5.3 | 98.6 | 102.4 | 92.5 |
250 | 3.9 | 94.2 | 5.6 | 100.9 | 100.8 | 91.8 | |
劳拉西泮 | 20 | 2.1 | 88.4 | 5.6 | 104.6 | 105.2 | 98.2 |
250 | 5.1 | 90.6 | 9.4 | 106.6 | 101.5 | 91.5 | |
咪达唑仑 | 1 | 4.9 | 97.3 | 7.1 | 94.8 | 98.2 | 92.5 |
250 | 2.7 | 100.9 | 8.5 | 97.7 | 103.5 | 86.9 | |
硝西泮 | 5 | 4.8 | 97.5 | 9.4 | 93.2 | 109.3 | 89.9 |
250 | 5.1 | 90.1 | 8.1 | 103.2 | 107.6 | 84.5 | |
7-氨基硝西泮 | 10 | 4.1 | 105.7 | 9.4 | 98.5 | 99.6 | 88.8 |
250 | 2.9 | 94.5 | 6.9 | 91.4 | 97.2 | 76.0 | |
唑吡坦 | 0.5 | 4.2 | 99.2 | 6.7 | 95.4 | 102.1 | 89.0 |
250 | 2.9 | 100.6 | 5.4 | 99.3 | 97.8 | 84.9 | |
西酞普兰 | 2 | 4.9 | 98.5 | 5.9 | 105.3 | 94.2 | 86.9 |
250 | 7.3 | 96.3 | 8.4 | 96.2 | 98.7 | 83.1 | |
苯海拉明 | 2 | 4.5 | 102.4 | 6.3 | 108.6 | 89.4 | 81.1 |
250 | 5.2 | 94.2 | 6.9 | 102.1 | 94.2 | 76.2 | |
右美沙芬 | 10 | 3.6 | 97.5 | 7.5 | 98.0 | 86.5 | 81.9 |
250 | 5.1 | 93.2 | 8.4 | 106.7 | 87.2 | 77.8 | |
氯氮平 | 2 | 1.9 | 98.2 | 6.0 | 99.4 | 91.6 | 87.2 |
250 | 4.2 | 97.2 | 5.5 | 93.8 | 94.2 | 81.7 | |
东莨菪碱 | 0.5 | 2.9 | 86.7 | 5.4 | 92.1 | 89.4 | 86.2 |
250 | 8.4 | 104.9 | 10.5 | 106.0 | 102.8 | 82.4 | |
右美托咪定 | 5 | 4.6 | 98.1 | 11.2 | 97.2 | 91.5 | 71.5 |
250 | 3.5 | 96.2 | 5.6 | 93.4 | 87.5 | 79.1 | |
曲马多 | 20 | 9.4 | 91.5 | 6.9 | 105.2 | 94.2 | 68.1 |
250 | 2.7 | 94.5 | 3.9 | 93.6 | 88.5 | 71.1 | |
安替比林 | 20 | 4.9 | 86.5 | 7.5 | 103.6 | 105.4 | 84.3 |
250 | 1.8 | 90.5 | 2.8 | 94.5 | 94.1 | 88.4 | |
卡马西平 | 5 | 2.1 | 98.4 | 5.7 | 97.9 | 102.7 | 75.4 |
250 | 3.8 | 98.2 | 7.8 | 96.3 | 97.5 | 82.6 | |
奥卡西平 | 10 | 3.6 | 97.1 | 9.3 | 96.5 | 100.2 | 89.4 |
250 | 4.2 | 102.9 | 6.5 | 100.1 | 104.6 | 79.2 | |
尼美西泮 | 2 | 5.1 | 98.2 | 8.8 | 96.8 | 88.9 | 87.2 |
250 | 4.6 | 101.7 | 6.7 | 105.5 | 89.4 | 84.9 | |
喹硫平 | 2 | 1.7 | 98.2 | 6.0 | 101.8 | 102.7 | 94.2 |
250 | 2.0 | 97.2 | 7.4 | 101.7 | 103.8 | 90.8 | |
米氮平 | 0.5 | 1.9 | 98.3 | 3.1 | 97.2 | 111.7 | 86.4 |
250 | 2.3 | 103.2 | 9.7 | 103.5 | 102.7 | 91.6 |
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