Introduction
Synthetic cannabinoids
Colorimetric detection
Immunochemical detection
GC–MS detection
LC–MS-MS detection
Target(s) | Sample(s) | Purification(s) | Column(s) | Mobile phase | LOD (ng/ml) | Linear range (ng/ml) | Reference(s) |
---|---|---|---|---|---|---|---|
JWH-018 | Serum | LLE | Luna C18 (2) (150 mm, 2 mm ID, 5 μm) (Phenomenex) | 10 mM ammonium acetate (0.1 % acetic acid, pH 3.2), methanol | 0.07 | 0.21–20 | [38] |
JWH-018, JWH-073, JWH-019, JWH-250 | Blood | LLE | Acquity UPLC HSS T3 (100 mm, 2.1 mm ID, 1.8 μm) (Waters) | 1 % formic acid, methanol (1 % formic acid) | 0.006–0.016 | 0.1–20 | |
Aminoalkylindoles, methanandamide | Serum | LLE | Luna phenyl hexyl (50 mm, 2 mm ID, 5 μm) (Phenomenex) | 2 mM ammonium formate (0.2 % formic acid), methanol | 0.1 | 0.1–2, 0.3–2 (methanandamide) | [41] |
JWH-018, JWH-073, metabolites | Urine | Dilution (hydrolysis) | Zorbax Eclipse XDB-C18 (150 mm, 4.6 mm ID, 5 μm) (Agilent) | 0.1 % formic acid, acetonitrile (0.1 % formic acid) | <2.0 | 2–100 | [42] |
Metabolites of JWH-018 and JWH-073 | Urine | SPE (hydrolysis) | Zorbax Eclipse XDB-C18 (150 mm, 4.6 mm ID, 5 μm) (Agilent) | 0.1 % formic acid/acetonitrile (0.1 % formic acid) (45:55), isocratic | <0.1 | 0.1–100 | [43] |
Metabolites of 8 synthetic cannabinoids | Urine | LLE (hydrolysis) | AQUASIL C18 (100 mm, 2.1 mm ID, 5 μm) (Thermo Scientific) | 5 mM ammonium acetate, methanol/acetonitrile (1:1, 5 mM ammonium acetate) | 0.1–10 | [44] | |
Metabolites of JWH-018 and JWH-073 | Urine | LLE (hydrolysis) | Acquity UPLC HSS T3 (100 mm, 2.1 mm ID, 1.8 μm) (Waters) | 0.1 % formic acid (0.1 %), acetonitrile (0.1 % formic acid) | 4–400 | [45] | |
30 Synthetic cannabinoids | Serum | LLE | Luna phenyl hexyl (50 mm, 2 mm ID, 5 μm) (Phenomenex) | 0.2 % formic acid (2 mM ammonium formate), methanol | 0.01–2.0 | 0.1–2.0 (2–40 : JWH-387) | |
Metabolites of 7 synthetic cannabinoids | Urine | LLE (hydrolysis) | Luna C18 (150 mm, 2 mm ID, 5 μm) (Phenomenex) | 0.2 % formic acid (2 mM ammonium formate), methanol | [49] | ||
22 Synthetic cannabinoids | Hair | Ethanol ext | Luna phenyl hexyl (50 mm, 2 mm ID, 5 μm) (Phenomenex) | 0.2 % formic acid (2 mM ammonium formate), methanol | 0.5 pg/mg | [37] | |
JWH-018, JWH-073 | Blood | LLE | Acquity UPLC BEH C18 (50 mm, 2.1 mm ID, 1.8 μm) (Waters) | 0.1 % formic acid, acetonitrile (0.1 % formic acid) | 0.01 | 0.05–50 | [50] |
UR-144, metabolites, pyrolysis product | Urine | LLE (hydrolysis) | Zorbax Eclipse XDB-C18 (150 mm, 2.1 mm ID, 3.5 μm) (Agilent) | 20 mM ammonium formate buffer (pH5), acetonitrile | [29] | ||
UR-144, metabolites | Blood, urine | PP | Kinetex C18 (100 mm, 4.6 mm ID, 2.6 μm) (Phenomenex), Ascentis express C18 (7.5 cm, 2.1 mm ID, 2.7 μm) (Supelco) | 0.1 % formic acid, acetonitrile (0.1 % formic acid) | 0.15 (blood) | 0.5–100 (blood) | [51] |
9 Synthetic cannabinoids, 20 metabolites | Urine | PP (hydrolysis) | XB-C18 (50 mm, 3.0 mm ID, 2.6 μm) (Kinetex) | 0.1 % formic acid, acetonitrile (0.1 % formic acid) | 0.5–10 | [34] | |
MAM-2201 | Blood | SPE | InertSustain C18 HP (100 mm, 3 mm ID, 3 μm) (GL Sciences) | 0.1 % acetic acid, acetonitrile | 1 | 2.5–100 | [52] |
5F-PB-22 | Blood, serum | LLE | Acquity UPLC BEH C18 (100 mm, 2.1 mm ID, 1.7 μm) (Waters) | 0.1 % formic acid, acetonitrile (0.1 % formic acid) | 0.1 | 0.5–10 | [53] |
Indole derivative synthetic cannabinoids | Saliva, urine, blood | PP (blood) LLE (urine, saliva) (hydrolysis) | Ascentis C18 (150 mm, 2.1 mm, 5 μm) (Supelco) | 0.1 % formic acid (5 mM ammonium formate), acetonitrile (0.1 % formic acid) | 0.1–0.5 | [54] |
Cathinones
Colorimetric detection
Immunochemical detection
GC–MS-MS detection
Target(s) | Sample(s) | Purification | Derivatization(s) | Column(s) | LOD(s) (ng/ml) | Linear range (ng/ml) | Reference |
---|---|---|---|---|---|---|---|
MDPV, metabolites | Urine | SPE (hydrolysis) | Methyl, acetyl, trimethylsilyl | HP-1 (12 m, 0.2 mm ID, 0.33 μm) (Agilent) | – | – | [68] |
MDPV, metabolites | Cellular fraction, urine | LLE (hydrolysis) | Trimethylsilyl | 5 % Phenyl-methylsilicone (17 m, 0.2 mm ID, 0.33 μm) (J and W) | 2 | 10–2,000 | [69] |
Mephedrone, MDPV | Blood, urine | LLE | DB-1 (30 m, 0.32 mm ID, 0.25 μm) (Agilent) | – | – | [70] | |
MDPV | Urine | LLE | Heptafluorobutyryl | HP-5MS (12 m, 0.2 mm ID, 0.33 μm) (Agilent), ZB-5MS (12 m, 0.2 mm ID, 0.33 μm) (Phenomenex) | 10 | 20–2,000 | [71] |
Methylone | Blood | LLE | Heptafluorobutyryl | RTx-5 MS (30 m, 0.25 mm ID, 0.25 μm) (Restek) | 50 | 100–2,000 | [72] |
α-PVP, pyrovalerone (PV), MDPV | Blood | SPME | InertCap 5 (30 m, 0.25 mm ID, 0.25 μm) (GL Sciences) | 0.5 (PV, PVP), 1.0 (MDPV) | 1–200 | [73] | |
MDPV, α-PVP, α-PBP | Blood | LLE (Extrelut) | InertCap 5MS/NP (30 m, 0.25 mm ID, 0.25 μm) (GL Sciences) | 1 | 2–2,000 | [74] | |
MDPV | Blood, tissue, urine | SPE | Zebron Guardian ZB-50 (10 m, 0.18 mm ID, 0.18 μm) (Phenomenex) | – | 10–2,000 | [75] | |
MDPV | Blood, urine | LLE | Rtx-5 ms (30 m, 0.25 mm ID, 0.25 μm) (Restek) | – | – | [76] | |
3,4-Dimethylmethcathinone, metabolites | Urine | LLE | Trifluoroacetyl | DB-5MS (30 m, 0.25 mm ID, 0.25 μm) (Agilent) | – | – | [77] |
16 Synthetic cathinones | Urine | LLE | Trifluoroacetyl | CP7684 (10 m, 0.15 mm ID, 0.12 μm) (Agilent) | – | – | [78] |
α-PVP, metabolites | Urine | LLE | Trimethylsilyl | DB-5MS (30 m, 0.25 mm ID, 0.25 μm) (Agilent) | – | – | [79] |
LC–MS-MS detection
Target(s) | Sample(s) | Purification(s) | Column(s) | Mobile phase(s) | LOD(s) (ng/ml or g) | Linear range (ng/ml or g) | Reference |
---|---|---|---|---|---|---|---|
MDPV, metabolites | Urine | SPE (hydrolysis) | Hypersil Gold column (10 mm, 2.1 mm ID, 1.9 μm) (Thermo Scientific) | 10 mM ammonium formate (0.1 % formic acid), acetonitrile (0.1 % formic acid) | [68] | ||
MDPV, metabolites | Cellular fraction, urine | LLE (hydrolysis) | Zorbax Eclipse Plus C18 (100 mm, 2.1 mm ID, 1.8 μm) (Agilent) | 0.1 % formic acid, acetonitrile (0.1 % formic acid) | [69] | ||
MDPV | Serum | SPE | Phenyl–hexyl (50 mm, 3.0 mm ID, 3 μm) (Phenomenex) | 10 mM ammonium acetate (0.1 % formic acid), methanol | 3 | 10–500 | [83] |
Mephedrone | Plasma | LLE | Synergi Fusion (150 mm, 4.6 mm ID)(Phenomenex); Spherisorb (150 mm, 4.6 mm ID) (Waters) | 10 % acetonitrile (25 mM triethylammonium phosphate buffer), isocratic | 39 | 78–10,000 | [84] |
9 Cathinones | Blood | PP | Prodigy Phenyl-3 (150 mm, 2.0 mm ID, 5 μm) (Phenomenex) | 0.1 % formic acid, methanol | 0.5–3 | 10–400 | [82] |
7 Cathinones | Hair | LLE | Kintex PFP (50 mm, 2 mm ID, 2.6 μm) (Phenomenex) | 5 mM ammonium formate (pH 3.5), methanol (5 mM ammonium formate) | 10–50 pg/mg | [85] | |
Butylone | Blood, liver | SPE | Allure PFP (50 mm, 2.1 mm ID, 5 μm) (Restek) | 0.02 % formic acid (2 mM of ammonium formate), acetonitrile | 25 (blood) | 50–2,000 (blood) | [86] |
4-Methylethcathinone | Blood, urine | LLE | Zorbax SB-C18 (50 mm, 2.1 mm ID, 1.8 μm) (Agilent) | 0.1 % formic acid, acetonitrile (0.1 % formic acid) | 0.96 (blood), 0.68 (urine) | 10–1,000 | [87] |
MDPV, α-PVP, α-PBP | Hair | LLE (Extrelut) | Phenyl-hexyl (150 mm, 2.1 mm ID, 3 μm) (Agilent) | 10 mM ammonium formate (0.1 % formic acid, pH 3.3)/methanol (65:35), isocratic | 0.02 ng/10-mm | 0.05–50 ng/10-mm | [74] |
Mephedrone | Blood | PP | Zorbax SB-C18 (50 mm, 2.1 mm ID, 1.8 μm) (Agilent) | 0.1 % formic acid, acetonitrile (0.1 % formic acid) | 0.08 | 1–100 | [88] |
MDPV, mephedrone | Blood, plasma, urine | SPE | Kintex PFP (50 mm, 2.1 mm ID, 1.8 μm) (Phenomenex) | 2 mM ammonium formate (2 % formic acid), acetonitrile (0.1 % formic acid) | 2 | 5–2,000 | [89] |
Mephedrone | Blood, urine | LLE | Zorbax SB-C18 (150 mm, 2.1 mm ID, 3.5 μm) (Agilent) | 0.1 % formic acid, methanol (0.1 % formic acid) | 1 (blood), 2 (urine) | 20–2,000 | [90] |
10 Cathinones | Blood, other specimens | LLE | Zorbax XDB-C18 (150 mm, 4.6 mm ID, 5 μm) (Agilent) | 5 mM ammonium acetate, methanol/acetonitrile | – | 5–200 | [91] |
MDPV | Hair | SPE | Zorbax Eclipse Plus C18 (50 mm, 2.1 mm, 1.8 μm) (Agilent) | 0.1 % formic acid, acetonitrile | 2.0 pg/mg | 2–3,000 pg/mg | [75] |
MDPV | Blood | PP | Zorbax SB-C18 (50 mm, 2.1 mm ID, 1.8 μm) (Agilent) | 0.1 % formic acid, acetonitrile (0.1 % formic acid) | 0.5 | 5–500 | [92] |
Buphedrone | Blood | PP | Zorbax SB-C18 (50 mm, 2.1 mm ID, 1.8 μm) (Agilent) | 0.1 % formic acid, acetonitrile (0.1 % formic acid) | 0.3 | 1–1,000 | [93] |
3,4-Dimethylmethcathinone, metabolites | Urine | PP (hydrolysis) | L-column2 ODS (150 mm, 1.5 mm ID, 5 μm) (Chemicals Evaluation and Research Institute) | 10 mM ammonium formate buffer (pH 5), methanol | – | 10–5,000 | [77] |
MDPV, metabolites | Plasma | PP (hydrolysis) | Synergy polar-RP (100 mm, 2 mm ID, 2.5 μm) (Phenomenex) | 0.1 % formic acid, acetonitrile (0.1 % formic acid) | 0.1 | 0.25–1,000 | [94] |
α-PBP | Blood, urine, tissues | QuEChERS | Zorbax Eclipse Plus C18 (100 mm, 2.1 mm ID, 1.8 μm) (Agilent) | 10 mM ammonium formate (0.1 % formic acid), acetonitrile | 0.05 (blood, urine), 0.1 (tissues) | 8.6–4,280 | [95] |
3,4-Dimethylmethcathinone, metabolites | Blood, urine | QuEChERS | Shim-pack XR-ODS III (50 mm, 2.0 mm ID, 1.6 μm) (Shimadzu); L-column2 ODS (150 mm, 1.5 mm ID, 5 μm) (Chemical Evaluation and Reaearch Institute) | 10 mM ammonium formate, methanol; 10 mM ammonium formate (pH 5.0), methanol | 1.03 (blood), 1.37 (urine) | 5–400 | [96] |
MDPV metabolittes | Urine | PP, LLE, SPE (hydrolysis) | Atlantis T3 (150 mm, 2.1 mm) (Waters) | 10 mM ammonium formate buffer (0.1 % formic acid), acetonitrile (0.1 % formic acid) | [97] | ||
α-PVP, metabolites | Urine | PP (hydrolysis) | L-column2 ODS (150 mm, 1.5 mm ID, 5 μm) (Chemicals Evaluation and Research Institute) | 10 mM ammonium formate (pH 5), methanol | – | 10–10,000 | [79] |
PV9 | Blood, urine | QuEChERS | Zorbax Eclipse Plus C18 (100 mm, 2.1 mm ID, 1.8 µm) (Agilent) | 10 mM ammonium formate (0.1 % formic acid), acetonitrile | 0.05 | 10–1,000 | [98] |