Journal of Forensic Medicine ›› 2024, Vol. 40 ›› Issue (3): 276-283.DOI: 10.12116/j.issn.1004-5619.2023.330802
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Jin-ting LIU1,2(), Li-ying ZHOU1, Jia-hong XIANG1, Zi-yi LI1, Wan-ting XIE1, Ke-ming YUN1,2, Yan SHI1(
)
Received:
2023-08-22
Online:
2024-08-20
Published:
2024-06-25
Contact:
Yan SHI
CLC Number:
Jin-ting LIU, Li-ying ZHOU, Jia-hong XIANG, Zi-yi LI, Wan-ting XIE, Ke-ming YUN, Yan SHI. Research Progress on Detection of New Psychoactive Substance Piperazines in vivo[J]. Journal of Forensic Medicine, 2024, 40(3): 276-283.
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URL: http://www.fyxzz.cn/EN/10.12116/j.issn.1004-5619.2023.330802
目标物 | 基质 | 样品处理 | 分析仪器 | 色谱条件 | 检出限/ (ng·mL-1) | 参考文献 |
---|---|---|---|---|---|---|
BZP | 血液 | LLE、衍生化 | GC-MS | HP-5MS(30 m×0.25 mm,0.25 μm),氦气0.9 mL/min,不分流模式 | - | [ |
BZP、TFMPP、mCPP、MeOPP、MDBP | 血液 | SPE、衍生化 | GC-MS | HP-5MS(30 m×0.25 mm,0.25 μm),氦气0.6 mL/min,不分流模式 | 5 | [ |
BZP、TFMPP、羟基化代谢产物 | 尿液 | LLE、SPE、衍生化 | GC-MS | DB-5MS(30 m×0.25 mm,0.25 μm),氦气1.0 mL/min,不分流模式 | - | [ |
mCPP | 尿液 | LLE、衍生化 | GC-MS | VF-5MS(30 m×0.25 mm,0.25 μm),氦气1.0 mL/min,不分流模式 | 16 | [ |
BZP、TFMPP | 尿液 | SPE、衍生化 | GC-MS | DB-5MS(20 m×0.18 mm,0.18 μm),氦气1.0 mL/min,分流模式(分流比10∶1) | - | [ |
BZP、羟基化代谢产物 | 尿液 | LLE、衍生化 | GC-MS | DB-5MS(30 m×0.25 mm,0.25 μm),氦气1 mL/min,不分流模式 | - | [ |
BZP | 尿液 | LLE、衍生化 | GC-MS | HP-5MS(30 m×0.25 mm,0.25 μm),氦气0.9 mL/min,不分流模式 | - | [ |
TFMPP、mCPP、MeOPP | 头发 | SPE | GC-MS | HP-5MS(30 m×0.25 mm,0.25 μm),氦气0.8 mL/min,分流模式(分流比5∶1) | - | [ |
mCPP | 血浆 | LLE | HPLC-DAD | LiChrospher 60 RP Select B(250 mm×5 mm,50 μm),流动相为V[0.02 mol/L磷酸缓冲液(pH=2)]∶V(乙腈)=36∶64,等度洗脱,流速为0.9 mL/min | - | [ |
BZP、TFMPP、羟基化代谢产物 | 血浆(鼠) | SPE | HPLC-FD | Daisopak-SP-ODS-BP(250 mm×4.6 mm,5 μm),流动相:A相为0.1 mol/L醋酸盐缓冲液(pH=3.5),B相为乙腈,梯度洗脱,流速为1.0 mL/min | 0.9;4.6 | [ |
BZP、TFMPP、羟基化代谢产物 | 尿液 | 酶解、LLE、SPE | LC-MS | SCX(2.0 mm×150 mm),流动相:V(40 mmol/L醋酸铵缓冲液)∶V(乙腈)=25∶75,等度洗脱,流速为0.15 mL/min | 5~40 | [ |
BZP、羟基化代谢产物 | 尿液 | SPE | HPLC-MS | SCX(2.0 mm×150 mm),流动相为V(40 mmol/L醋酸铵缓冲液)∶V(乙腈)=25∶75,等度洗脱,流速为0.15 mL/min | - | [ |
BZP、TFMPP | 尿液 | LLE | HPLC-MS | Polar-RP C18(2.0 mm×150 mm,4 mm),流动相:A相为0.1%甲酸,B相为乙腈,梯度洗脱,流速为0.4 mL/min | 100 | [ |
BZP、TFMPP、羟基化代谢产物 | 血液 | 硫酸盐、甲醇沉淀蛋白 | HPLC-MS | Zorbax C18(4.6 mm×150 mm,5 μm),流动相:A相为0.01 mol/L甲酸铵缓冲液(pH=4.5),B相为乙腈,梯度洗脱,流速为1.0 mL/min | - | [ |
BZP | 头发 | SPE | HPLC-MS/MS | SCX(2.0 mm×150 mm),流动相为V[甲酸铵(100 mmol/L)]∶V(0.5 %甲酸-乙腈)=25∶75,等度洗脱,流速为0.2 mL/min | - | [ |
BZP、TFMPP、mCPP、MeOPP、MDBP | 血液 | SPE | HPLC-MS/MS | Synergi Polar RP(150 mm×2 mm,4 μm),流动相:A相为1 mmol/L甲酸铵-0.1%甲酸,B相为0.1%甲酸-甲醇,梯度洗脱,流速为0.25mL/min | 1~5 | [ |
BZP、TFMPP、mCPP | 血液 | LLE | UHPLC-MS/MS | ACQUITY UPLC T3(2.1 mm×50 mm,1.8 μm),流动相:A相为0.1%甲酸水,B相为乙腈,梯度洗脱,流速为0.6 mL/min | 0.04~0.13 | [ |
Tab. 1 Methods for the analysis of piperazines NPS in vivo
目标物 | 基质 | 样品处理 | 分析仪器 | 色谱条件 | 检出限/ (ng·mL-1) | 参考文献 |
---|---|---|---|---|---|---|
BZP | 血液 | LLE、衍生化 | GC-MS | HP-5MS(30 m×0.25 mm,0.25 μm),氦气0.9 mL/min,不分流模式 | - | [ |
BZP、TFMPP、mCPP、MeOPP、MDBP | 血液 | SPE、衍生化 | GC-MS | HP-5MS(30 m×0.25 mm,0.25 μm),氦气0.6 mL/min,不分流模式 | 5 | [ |
BZP、TFMPP、羟基化代谢产物 | 尿液 | LLE、SPE、衍生化 | GC-MS | DB-5MS(30 m×0.25 mm,0.25 μm),氦气1.0 mL/min,不分流模式 | - | [ |
mCPP | 尿液 | LLE、衍生化 | GC-MS | VF-5MS(30 m×0.25 mm,0.25 μm),氦气1.0 mL/min,不分流模式 | 16 | [ |
BZP、TFMPP | 尿液 | SPE、衍生化 | GC-MS | DB-5MS(20 m×0.18 mm,0.18 μm),氦气1.0 mL/min,分流模式(分流比10∶1) | - | [ |
BZP、羟基化代谢产物 | 尿液 | LLE、衍生化 | GC-MS | DB-5MS(30 m×0.25 mm,0.25 μm),氦气1 mL/min,不分流模式 | - | [ |
BZP | 尿液 | LLE、衍生化 | GC-MS | HP-5MS(30 m×0.25 mm,0.25 μm),氦气0.9 mL/min,不分流模式 | - | [ |
TFMPP、mCPP、MeOPP | 头发 | SPE | GC-MS | HP-5MS(30 m×0.25 mm,0.25 μm),氦气0.8 mL/min,分流模式(分流比5∶1) | - | [ |
mCPP | 血浆 | LLE | HPLC-DAD | LiChrospher 60 RP Select B(250 mm×5 mm,50 μm),流动相为V[0.02 mol/L磷酸缓冲液(pH=2)]∶V(乙腈)=36∶64,等度洗脱,流速为0.9 mL/min | - | [ |
BZP、TFMPP、羟基化代谢产物 | 血浆(鼠) | SPE | HPLC-FD | Daisopak-SP-ODS-BP(250 mm×4.6 mm,5 μm),流动相:A相为0.1 mol/L醋酸盐缓冲液(pH=3.5),B相为乙腈,梯度洗脱,流速为1.0 mL/min | 0.9;4.6 | [ |
BZP、TFMPP、羟基化代谢产物 | 尿液 | 酶解、LLE、SPE | LC-MS | SCX(2.0 mm×150 mm),流动相:V(40 mmol/L醋酸铵缓冲液)∶V(乙腈)=25∶75,等度洗脱,流速为0.15 mL/min | 5~40 | [ |
BZP、羟基化代谢产物 | 尿液 | SPE | HPLC-MS | SCX(2.0 mm×150 mm),流动相为V(40 mmol/L醋酸铵缓冲液)∶V(乙腈)=25∶75,等度洗脱,流速为0.15 mL/min | - | [ |
BZP、TFMPP | 尿液 | LLE | HPLC-MS | Polar-RP C18(2.0 mm×150 mm,4 mm),流动相:A相为0.1%甲酸,B相为乙腈,梯度洗脱,流速为0.4 mL/min | 100 | [ |
BZP、TFMPP、羟基化代谢产物 | 血液 | 硫酸盐、甲醇沉淀蛋白 | HPLC-MS | Zorbax C18(4.6 mm×150 mm,5 μm),流动相:A相为0.01 mol/L甲酸铵缓冲液(pH=4.5),B相为乙腈,梯度洗脱,流速为1.0 mL/min | - | [ |
BZP | 头发 | SPE | HPLC-MS/MS | SCX(2.0 mm×150 mm),流动相为V[甲酸铵(100 mmol/L)]∶V(0.5 %甲酸-乙腈)=25∶75,等度洗脱,流速为0.2 mL/min | - | [ |
BZP、TFMPP、mCPP、MeOPP、MDBP | 血液 | SPE | HPLC-MS/MS | Synergi Polar RP(150 mm×2 mm,4 μm),流动相:A相为1 mmol/L甲酸铵-0.1%甲酸,B相为0.1%甲酸-甲醇,梯度洗脱,流速为0.25mL/min | 1~5 | [ |
BZP、TFMPP、mCPP | 血液 | LLE | UHPLC-MS/MS | ACQUITY UPLC T3(2.1 mm×50 mm,1.8 μm),流动相:A相为0.1%甲酸水,B相为乙腈,梯度洗脱,流速为0.6 mL/min | 0.04~0.13 | [ |
案例 | 案例摘要 | 毒(药)物检验结果 | 文献 |
---|---|---|---|
1 | 23岁女性,出现心律失常、高血压、意识部分丧失等中毒症状,后死于脑水肿 | 血液中检出BZP和MDMA | [ |
2 | 20岁男性,口服4片“Rapture”,出现精神障碍、幻听和幻视 | 血液中检出BZP | [ |
3 | 23岁女性,口服3粒“Party-Pills”,出现激动、幻视和心动过速 | 血浆中检出mCPP 320 ng/mL、乙醇0.7 mg/mL、苯丙胺40 ng/mL、苯甲酰爱康宁47 ng/mL,尿液中检出mCPP 2 300 ng/mL | [ |
4 | 3名18~19岁男性,分别口服4片“Ecstasy”,出现恶心、解离症状、激动、心律失常等症状 | 血清中检出BZP 260~270 ng/mL、TFMPP 30~60 ng/mL | [ |
5 | 23岁女性,出现阵发性痉挛、心动过速、高热、呼吸急促等症状 | 血浆中检出BZP 200 ng/mL,尿液中检出苯扎托品、咖啡因和尼古丁的代谢物 | [ |
6 | 22岁男性,口服4粒“Party-Pills”,出现肌肉强直、激动、心动过速和昏迷等症状 | 血液中检出BZP 2 230 ng/mL,MDMA 1 050 ng/mL | [ |
7 | 16岁女性,口服3粒“Party-Pills”,出现肌肉强直、癫痫等症状,送至医院急诊后反复发作 | 尿液中检出BZP及其代谢产物 | [ |
Tab. 2 Typical cases of misuse of piperazines NPS mixed with other poisons (drugs)
案例 | 案例摘要 | 毒(药)物检验结果 | 文献 |
---|---|---|---|
1 | 23岁女性,出现心律失常、高血压、意识部分丧失等中毒症状,后死于脑水肿 | 血液中检出BZP和MDMA | [ |
2 | 20岁男性,口服4片“Rapture”,出现精神障碍、幻听和幻视 | 血液中检出BZP | [ |
3 | 23岁女性,口服3粒“Party-Pills”,出现激动、幻视和心动过速 | 血浆中检出mCPP 320 ng/mL、乙醇0.7 mg/mL、苯丙胺40 ng/mL、苯甲酰爱康宁47 ng/mL,尿液中检出mCPP 2 300 ng/mL | [ |
4 | 3名18~19岁男性,分别口服4片“Ecstasy”,出现恶心、解离症状、激动、心律失常等症状 | 血清中检出BZP 260~270 ng/mL、TFMPP 30~60 ng/mL | [ |
5 | 23岁女性,出现阵发性痉挛、心动过速、高热、呼吸急促等症状 | 血浆中检出BZP 200 ng/mL,尿液中检出苯扎托品、咖啡因和尼古丁的代谢物 | [ |
6 | 22岁男性,口服4粒“Party-Pills”,出现肌肉强直、激动、心动过速和昏迷等症状 | 血液中检出BZP 2 230 ng/mL,MDMA 1 050 ng/mL | [ |
7 | 16岁女性,口服3粒“Party-Pills”,出现肌肉强直、癫痫等症状,送至医院急诊后反复发作 | 尿液中检出BZP及其代谢产物 | [ |
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