Table 1.
A comparison of the various conditions of the MMPB method protocols in scientific publications (modified after Anaraki et al. [87]). (n.s.: not specified; dw: dry weight).
| References | Matrix | Quantity of Matrices | Pre-Treatment Step | Oxidation Length (Hour) | [KMnO4] | [NaIO3] or [NaIO4] | pH | End of Reaction | Purification Method | Detection Limits | Instrumental Analysis | Yield | |
|---|---|---|---|---|---|---|---|---|---|---|---|---|---|
| Sano et al. [65] | MC fraction from waterblooms (Microcystis viridis) | 0.2–1 mg (dw) | - | 4 | 0.024 M | 0.02 M | n.s. | 0.04 mL of 20% NaHSO₃ + 0.01 mL of 1OM H2SO4 | 5 mL of ethyl acetate | pmol | GC-FID/HPLC | 84–98% | |
| Williams et al. [60] | Salmon Liver (Salmo salar) | 220–1366 mg | - | overnight | 36.1 µM | 1.3852 mM | 9 (120.8 µM of K2CO3) | NaHSO₃ + 10% H2SO4 (pH~2) | Diethyl ether | 15 µg/g | GC/MS | 85–95% | |
| Dungeness Crab Larvae (Cancer magister) | 5.2–5.4 g | n.s. | |||||||||||
| Williams et al. [71] | Saltwater mussels, (Mytilus edulis) | 5.5–8.3 g | - | n.s. | 334.2 µM | 12.3 mM | 9 | NaHSO₃ + 10% H2SO4 (pH ≈ 1–2 | Diethyl ether | 15 µg/g | GC/MS | n.s. | |
| Pires et al. [93] | Zebra mussels (Dreissena polymorpha) | Pooled mussel material | - | overnight | 0.1 M | 0.4 M | 9 | H2SO4 (1 M), pH < 3 | C18 (Supelco) | n.s. | LC/MS | n.s. | |
| Ott and Carmichael [72] | Rat or chicken livers (species n.s.) | 0.5–1 g | - | 3 | 0.02 M | 0.02 M | 9 (KHCO3) | 0.5–1.5 g of NaHSO₃ + 10% H2SO4 (pH ≈ 2) | 3 M Empore SDB-XC 7 mm/3 mL (Fischer Scientific, Hampton, NH, USA) | 5 µg/g | LC/MS | 33.5% | |
| Soares et al. [74] | Human sera | 0.4–1 mL | - | 3 | 0.02 M | 0.02 M | 9 (KHCO3) | 0.5–1.5 g of NaHSO₃ + 10% H2SO4 (pH ≈ 2) | 3 M Empore SDB-XC 7 mm/3 mL (Fischer Scientific) | n.s | LC/MS | n.s. | |
| Yuan et al. [75] | Human Liver/sera | n.s. | - | 3 | 0.02 M | 0.02 M | 9 (KHCO3) | 0.5–1.5 g of NaHSO₃ + 10% H2SO4 (pH ≈ 2) | 3 M Empore SDB-XC 7 mm/3 mL (Fischer Scientific) | n.s. | GC/MS | n.s. | |
| Hilborn et al. [73] | Human blood | n.s. | - | 3 | 0.02 M | 0.02 M | 9 (KHCO3) | 0.5–1.5 g of NaHSO₃ + 10% H2SO4 (pH ≈ 2) | 3M Empore SDB-XC 7 mm/3 mL (Fischer Scientific) | n.s | LC/MS | n.s. | |
| Nasri et al. [76] | Terrapin (E. orbicularis; M. leprosa) | 100 mg (dw) | - | 3 | 0.02 M | 0.02 M | 9 (KHCO3) | 0.5–1.5 g of NaHSO₃ + 10% H2SO4 (pH ≈ 2) | Conversion of MMPB to methyl ester using 12% trifluoroborate in MeOH | n.s. | GC/MS | n.s. | |
| Wu et al. [90] | Aqueous solution spiked with MC-LR | - | - | hours | 50 mg/L | 20 mg/L | 1.6 | NaHSO₃ | - | n.s. | HPLC/DAD | ~90% | |
| Wu et al. [67] | Cyanobacterial samples (Microcystis spp.) | 10; 20; 40; 60; 80; 100 mg (dw) | - | 1–4 | ≥0.05 M | 0.2 M | 9 (KHCO3) | Saturated NaHSO₃ sol. | - | n.s | LC/DAD | 86.7% | |
| Lance et al. [28], Neffling et al. [49] | Tissues of snails (Lymnaea stagnalis) | 10 mg (freeze-dried) | Trypsin in Sörensen’s phosphate buffer (0.5 mg/mL, pH 7.5, 37 °C) | 3 | 0.1 M | 0.1 M | 9 | 40% NaHSO₃ + 10% H2SO4 | Oasis HLB 30 mg | n.s. | LC/MS | 16–37% | |
| Suchy and Berry [61] | Rainbow Trout (Oncorhynchus mykiss) liver slurry (7 g in 5 mL of deionized water) | 1 mL of liver slurry | - | 3 | 0.0035 M | 0.09 M | 9 | 0.5–1.5 g of NaHSO₃ + 10% H2SO4 (pH ≈ 2) | Solid phase microextraction (PDMS-DVB fibre) | 0.04 µg/g | GC/MS | n.s. | |
| Wu et al. [69] | Lake sediment | 2 g (freeze dried) | - | 1–4 | 0.05 M | 0.1 M | 9 | Saturated NaHSO₃ sol. | Sep-pak C18 500 mg (Waters) | n.s. | HPLC/DAD | 33-45% | |
| Bieczynski et al. [81] | Supernatants of liver and intestines from fish (Odontesthes hatcheri) | 1 g | - | overnight | 0.002 M | 0.007 M | 9 | 20% NaHSO₃ + drops of 10% H2SO4 | Diethyl ether | 0.2 ng | GC/MS | 67.25 ± 26% | |
| Cadel-Six et al. [29] | Rainbow trout (Oncorhynchus mykiss) | Liver Intestines Gill Filet |
60 mg 100 mg 100 mg 100 mg (dw) |
Trypsin in Sörensen’s phosphate buffer (0.5 mg/mL, pH 7.5, 37 °C) | 4 | 0.1 M | 0.1 M | 9 | 40% NaHSO₃ + 10% H2SO4 (pH ≈ 1.5) | SampliQ OPT 150 mg (Agilent) | 2.59 ng/g 4.76 ng/g 2.86 ng/g 2.88 ng/g |
LC/MS | 17% 6% 12% 5% |
| Roy-Lachapelle et al. [66] | River water | n.s. | - | 1 | 0.05 M | 0.05 M | 9 (K2CO3) | 40% NaHSO₃ + 10% H2SO4 (pH ≈ 2) | Ethyl acetate | 0.2 µg/L | LDTD/APCI/MS | 91% | |
| Roy-Lachapelle et al. [79] | Frozen homogenized fish tissue ((Osmerus mordax); (Mugil cephalus); (Salvelinus fontinalis); (Perca flavescens); (Sander vitreus); (Ameiurus nebulosus); (Coregonus clupeaformis)) | 1 g | 3 freeze-thaw lysis cycles + 2 h in NaOH (50 mM) | 2 | 0.05 M | 0.05 M | 9 (HCl, 50 mM) | Saturated NaHSO₃ sol. + 10% H2SO4 (pH ≈ 2) | Filter the supernatants with 0.2 µM nylon filter (Whatman) + Strata SDB-L 500 mg (Phenomenex) | 2.7 ng/g | LDTD/APCI/HRMS | 54–72% | |
| Foss and Aubel [63] | Raw and trated water from Ohio water sources | n.s. | 3 freeze-thaw cycles + 10/100x concentration (SPE) | 0.5 | 0.015 M | 0.015 M | n.s. | 40% NaHSO₃ + phosphate buffer to raise pH < 5 | Strata X 100 mg (Phenomenex) | 0.05 µg/L | LC/MS | n.s. | |
| Wang et al. [68] | Water Sediment |
0.1 mL 1 g |
- | 1 | 4 g/L | 20 mg/L | n.s. | 40% NaHSO₃ (50 µL: water/0.5 mL: sediment) | Sep-Pak cartridge (500 mg, 6 cm3) | 125 ng/L 100 ng/g |
HPLC/FLD | 98–109% | |
| Greer et al. [77] | Tilapia (O. niloticus) filets, livers and eggs | 50 mg (dw) | - | 2 | 0.1 M | 0.1 M | n.s. | 40% NaHSO₃ + 10% H2SO4 (pH ≈ 2) | Oasis PRiME 60 mg (Waters) | n.s. | UPLC/MS | 55% | |
| Munoz et al. [64] | Surface Water | 10 mL | 3 freeze-thaw cycles + filtration (0.22 µM nylon filters) | 1 | 0.35 M | 0.4 M | 9 (K2CO3, 1 M) | NaHSO₃ (4 M) | Filtration (0.22 µM nylon filters) + on-line SPE | 0.5 ng/L | LC/MS | 65% | |
| Roy-Lachapelle et al. [80] | Algary dietary supplements | 0.3 g | - | 2 | 0.05 M | 0.05 M | 9 (K2CO3) | Saturated NaHSO₃ sol. + 10% H2SO4 (pH ≈ 2) | Filtration (0.2 µM nylon filter, Whatman) + Strata SDB-L 500 mg (Phenomenex) | 0.2 µg/g | LDTD/APCI/HRMS | 67–74% | |
| Vudathala et al. [94] | Liver and plasma from channel catfish (Ictalurus punctatus) | <0.5 g/0.08–0.18 g | - | 3 | 0.002 M | 0.002 M | 9 (Na2CO3, 1 M) | NaHSO₃ + 0.5 mL of concentrated H2SO4 (pH ≤ 2) | Filtration (0.2 µM nylon filter, Whatman) + Oasis HLB 60 mg (Waters) | 5.2–6.2 ng/g | LC/MS | 31%/21% | |
| Brown et al. [78] | Bottlenose dolphins liver (T. truncatus) | n.s. | - | 2.5 | 0.1 M | 0.1 M | n.s. (K2CO3, 0.2 M) | 40% NaHSO₃ | Strata-X 200 mg (Phenomenex) | 1.3 µg/g (dw) | LC/MS | 39% | |
| Duncan et al. [88] | Aqueous samples/Algal reference material suspensions | n.s./25 mg (dw) in 200 mL of water | - | 1.5 | 0.025 M | 0.009 M | 9 (KHCO3, 0.5 M) | 40% NaHSO₃ + HCl (6 M, pH ≈ 3) | Semi-permeable hydrophobic membrane (PDMS) |
1 µg/L | CP/MIMS | n.s. | |
| Foss et al. [59] | Mallard duck (Anas platyrhynchos) liver | 100 mg (dw) | - | 2 | 0.25 M | 0.25 M | KHCO3 (1 M) | 40% NaHSO₃ + 50% H2SO4 (pH < 2) | Ethyl acetate + Strata-X 200 mg (Phenomenex) | n.s. | LC/MS | n.s. | |
| Greer et al. [95] | Porcine tissue | 50 mg (dw) | - | 2 | 0.1 M | 0.2 M | n.s. | 40% NaHSO3 + 10% H2SO4 | Oasis PRiME HLB (Waters) | n.s. | UPLC/MS | 83% | |
| Foss et al. [86] | Dogs (Canis lupus familiaris) | Liver Kidney Hair Blood Bile Urine Vomit |
100 mg 100 mg 50 mg (dw) 0.5–1.5 mL 0.2–500 µL 0.2–500 µL 10 mg |
- | 2 | 0.1 M | 0.1 M | (K2CO3, 0.2 M) | 40% NaHSO₃ | Strata-X 200 mg (Phenomenex) + filtration (PVDF; 0.2 µM; Sigma) | 4 ng/g 4 ng/g 20 ng/g 0.2 ng/mL 50 ng/mL 0.2 ng/mL n.s. |
LC/MS | 21% 12% 4% 28% 72% 42% 114% |
| Mohamed et al. [5] | Nile tilapia (Oreochromis niloticus) filet |
n.s. | As described in Neffling et al. [49] | n-hexane | n.s. | LC/DAD | n.s. | ||||||
| Anaraki et al. [87] | Rainbow Trout (O. mykiss) liver and filet |
100 mg (dw) | - | 2 | 0.3 mM | 0.02 M | 8.5 | NaHSO₃ + 10% H2SO4 (pH = 3) | Oasis HLB 400 mg (Waters) + Pall GHP filters | 7.28 ng/g | LC/MS | 30% | |
| Bolotaolo et al. [70] | Sediments/clams | 1/0.1 g (dw) | - | 3 | 0.1 M | 0.1 M | 9 | NaHSO₃ (1–1.5 g) + 10% H2SO4 (pH = 2) | ENV-Bond Elut 100 mg (Agilent) + esterification | 10/15 ng/g (dw) | GC/MS | 50%/46% | |
| Lepoutre et al. [83] | Mussels (A. anantina and D. polymorpha) | Freeze-dried tissues | Trypsin in Sörensen’s phosphate buffer (pH 7.5, 37 °C) | 3 | 0.025 M | 0.025 M | 9 | NaHSO₃ + 10% H2SO4 (pH < 3) | SPE 60 mg (Waters) | n.s. | LC-MS/MS | 32.9–58.8/36.5–57% | |