Research Progress on the Analysis of Anabolic Androgenic Steroids in Biological Samples Based on High Resolution Mass Spectrometry

doi:10.12116/j.issn.1004-5619.2024.340705

Abstract

Abstract:

Anabolic androgenic steroids （AASs） are a class of synthetic steroid hormones that mimic androgens, and they rank as the most widely abused doping agents worldwide. High resolution mass spectrometry （HRMS） has unique advantages in the detection of AASs due to its high resolution, high sensitivity, high selectivity and data traceability. HRMS can not only be used for the qualitative and quantitative analysis of AASs and their metabolites in different biological samples, effectively improving the ability to analyze complex samples and increasing the reliability of analytical results, but can also infer AASs metabolites and reveal metabolic pathways by combining in vitro and in vivo metabolic models. This paper reviews the research progress of HRMS in AASs analysis methods, in vitro and in vivo metabolism of AASs, and also explores its application prospects in the field of forensic science.

Key words: forensic medicine, toxicological analysis, high resolution mass spectrometry （HRMS）, anabolic androgenic steroid, doping agent, biological sample, metabolite, review

CLC Number:

Zhen-shuo GUO, Wen-jia DUAN, Yu LIU, Yi-ling TANG, Hui YAN. Research Progress on the Analysis of Anabolic Androgenic Steroids in Biological Samples Based on High Resolution Mass Spectrometry[J]. Journal of Forensic Medicine, 2024, 40(6): 533-541.

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References 49

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编号	目标物	样本	前处理方法	检测方法	LOD	文献
1	21种AAS及其酯（氯司替勃、孕三烯酮、四氢孕三烯酮等）	尿液	稀释注射法	LC-Orbitrap-HRMS	0.5~18 ng/mL	[13]
2	司坦唑醇	尿液	稀释注射法联合在线固相萃取	UPLC-Orbitrap-HRMS	75 pg/mL	[14]
3	11种AAS（前列他唑、依西美坦、美曲勃龙等）	尿液	液液萃取	LC-Orbitrap-HRMS	0.05~0.5 ng/mL	[15]
4	70种AAS及其酯（勃地酮、卡芦睾酮、达那唑等）	尿液	液液萃取	GC-Orbitrap-HRMS	0.1~1.25 ng/mL	[16]
5	8种AAS（睾酮、表睾酮、雄诺龙等）	血液	固相萃取	UPLC-Orbitrap-HRMS	0.006~7.904 ng/mL	[17]
6	7种AAS（普拉睾酮、美雄醇、雄烯二醇等）	尿液、头发	中空纤维溶剂-搅拌棒微萃取装置	GC-Orbitrap-HRMS	尿液<0.1 ng/mL，头发<0.1 ng/mL	[18]
7	睾酮、普拉睾酮、雄诺龙等	头发	固相萃取和液液萃取	UPLC-Orbitrap-HRMS	0.3~3.5 pg/mg	[19]
8	41种AAS及其酯（屈他雄酮丙酸酯、诺乙雄龙、宝丹酮醋酸酯等）	马毛	液液萃取	UPLC-Orbitrap-HRMS	除癸酸诺龙（15.7 pg/mg）、癸酸睾酮（15.7 pg/mg）和屈他雄酮丙酸酯（32.5 pg/mg）外，其余为0.2~10 pg/mg	[20]
9	司坦唑醇	体毛（头发、腋毛、腿毛等）	液液萃取	UPLC-Q-TOF-HRMS	2 pg/mg	[21]
10	勃地酮、美雄酮、美雄醇、司坦唑醇等	干血斑	液液萃取	LC-Orbitrap-HRMS	0.03~2.25 ng/mL	[22]
11	13种AAS（环戊丙酸睾酮、十一酸睾酮和异丁酸睾酮等）	干血斑	DBSA-TLX-HRMS系统	LC-Orbitrap-HRMS	0.2~0.5 ng/mL	[23]
12	4种睾酮酯（癸酸睾酮、异己酸睾酮、苯丙酸睾酮和丙酸睾酮）	干血斑	液液萃取	nanoLC-Orbitrap-HRMS	50~200 pg/mL	[24]
13	依诺波沙	指甲、头发	液液萃取	LC-Orbitrap-HRMS	均为0.5 pg/mg	[25]
14	司坦唑醇	猪血浆、猪精液	液液萃取	LC-Orbitrap-HRMS	猪血浆：0.02~0.40 ng/mL；猪精液：0.01~0.25 ng/mL	[26]

编号	目标物	样本	前处理方法	检测方法	LOD	文献
1	21种AAS及其酯（氯司替勃、孕三烯酮、四氢孕三烯酮等）	尿液	稀释注射法	LC-Orbitrap-HRMS	0.5~18 ng/mL	[13]
2	司坦唑醇	尿液	稀释注射法联合在线固相萃取	UPLC-Orbitrap-HRMS	75 pg/mL	[14]
3	11种AAS（前列他唑、依西美坦、美曲勃龙等）	尿液	液液萃取	LC-Orbitrap-HRMS	0.05~0.5 ng/mL	[15]
4	70种AAS及其酯（勃地酮、卡芦睾酮、达那唑等）	尿液	液液萃取	GC-Orbitrap-HRMS	0.1~1.25 ng/mL	[16]
5	8种AAS（睾酮、表睾酮、雄诺龙等）	血液	固相萃取	UPLC-Orbitrap-HRMS	0.006~7.904 ng/mL	[17]
6	7种AAS（普拉睾酮、美雄醇、雄烯二醇等）	尿液、头发	中空纤维溶剂-搅拌棒微萃取装置	GC-Orbitrap-HRMS	尿液<0.1 ng/mL，头发<0.1 ng/mL	[18]
7	睾酮、普拉睾酮、雄诺龙等	头发	固相萃取和液液萃取	UPLC-Orbitrap-HRMS	0.3~3.5 pg/mg	[19]
8	41种AAS及其酯（屈他雄酮丙酸酯、诺乙雄龙、宝丹酮醋酸酯等）	马毛	液液萃取	UPLC-Orbitrap-HRMS	除癸酸诺龙（15.7 pg/mg）、癸酸睾酮（15.7 pg/mg）和屈他雄酮丙酸酯（32.5 pg/mg）外，其余为0.2~10 pg/mg	[20]
9	司坦唑醇	体毛（头发、腋毛、腿毛等）	液液萃取	UPLC-Q-TOF-HRMS	2 pg/mg	[21]
10	勃地酮、美雄酮、美雄醇、司坦唑醇等	干血斑	液液萃取	LC-Orbitrap-HRMS	0.03~2.25 ng/mL	[22]
11	13种AAS（环戊丙酸睾酮、十一酸睾酮和异丁酸睾酮等）	干血斑	DBSA-TLX-HRMS系统	LC-Orbitrap-HRMS	0.2~0.5 ng/mL	[23]
12	4种睾酮酯（癸酸睾酮、异己酸睾酮、苯丙酸睾酮和丙酸睾酮）	干血斑	液液萃取	nanoLC-Orbitrap-HRMS	50~200 pg/mL	[24]
13	依诺波沙	指甲、头发	液液萃取	LC-Orbitrap-HRMS	均为0.5 pg/mg	[25]
14	司坦唑醇	猪血浆、猪精液	液液萃取	LC-Orbitrap-HRMS	猪血浆：0.02~0.40 ng/mL；猪精液：0.01~0.25 ng/mL	[26]

编号	目标物	样本类型	检测方法	检测结果	文献
1	19-去甲睾酮	尿液	IRMS-GC-Q-TOF-HRMS	Ⅰ相代谢物10个：M1~M10；Ⅱ相代谢物11个：M11~M21	[40]
2	群勃龙	尿液	IRMS-LC-Q-TOF-HRMS	20种代谢物，包括葡萄糖醛酸酯、硫酸酯和潜在的半胱氨酸偶联物	[41]
3	司坦唑醇	斑马鱼	LC-Orbitrap-HRMS	4种葡萄糖醛酸酯代谢物和4种硫酸酯代谢物	[42]
4	勃拉睾酮	大鼠肝微粒体、血液	LC-Orbitrap-HRMS	Ⅰ相代谢物17个：M1~M17；Ⅱ相代谢物1个：M18	[43]
5	甲基司腾勃龙	马肝微粒体、尿液、血液	UPLC-Orbitrap-HRMS	体外肝微粒体：6种代谢物；体内尿液和血液：共14种代谢物	[44]
6	7-羰基-普拉睾酮	尿液	IRMS-GC-Q-TOF-HRMS	10种Ⅰ相代谢物以不同形式与葡萄糖醛酸酯和硫酸酯结合排出体外	[45]

编号	目标物	样本类型	检测方法	检测结果	文献
1	19-去甲睾酮	尿液	IRMS-GC-Q-TOF-HRMS	Ⅰ相代谢物10个：M1~M10；Ⅱ相代谢物11个：M11~M21	[40]
2	群勃龙	尿液	IRMS-LC-Q-TOF-HRMS	20种代谢物，包括葡萄糖醛酸酯、硫酸酯和潜在的半胱氨酸偶联物	[41]
3	司坦唑醇	斑马鱼	LC-Orbitrap-HRMS	4种葡萄糖醛酸酯代谢物和4种硫酸酯代谢物	[42]
4	勃拉睾酮	大鼠肝微粒体、血液	LC-Orbitrap-HRMS	Ⅰ相代谢物17个：M1~M17；Ⅱ相代谢物1个：M18	[43]
5	甲基司腾勃龙	马肝微粒体、尿液、血液	UPLC-Orbitrap-HRMS	体外肝微粒体：6种代谢物；体内尿液和血液：共14种代谢物	[44]
6	7-羰基-普拉睾酮	尿液	IRMS-GC-Q-TOF-HRMS	10种Ⅰ相代谢物以不同形式与葡萄糖醛酸酯和硫酸酯结合排出体外	[45]

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