Table 3.
Chromatographic methods for determination of nitrosamines.
| Matrix | Compounds | Sample Preparation | Analytical Instruments | Analytical Column | Detector | LOD | LOQ | RSD (%) | Recovery (%) | Reference |
|---|---|---|---|---|---|---|---|---|---|---|
| River Water | NDMA, NDEA, NDPA, NMEA, NDBA, NDPHA NDMA–d6 |
SPE (CCC) Restek (cat. #26032). USEPA Method 521 | GC Agilent 6890 N |
Rtx 5SiL MS (30 m × 0.25 mm ID × 1.0 μm). | Agilent MS 5973. |
2.5–40.6 ng/L | 7.9–127.7 ng/L | <15 | 72.3–98.6 | [54] |
| Potable water | NDMA-d6NDMA, NDPA, NPIP, NMEA, NDEA, NPYR, NDBA, | SPE (CCC) Restek (cat. #26032). USEPA Method | GC (TQ8030 Shimadzu) | 35 m × 0.25 mm x 0.5 μm. Restek Rxi 5Sil MS | MS (TQ8030 (Shimadzu) | 1.2–9.0 ng/L | NR | <20 | 70–130 | [55] |
| Tap & River water | DMA, EMA, DEA, DPA, TMA, DMAI. DMAPI. | No preconcentration steps. Filtered through (0.22 mm) |
UFLC (Shimadzu LC-20ADXR) | ThecolumnwasaPhenomenex Polar-RPC-18 column (150× 2.0 mmI.D,4 mm particlesize, | TMS (A 4000Q, AB SCIEX, Concord) | 0.02–1 μg/L | NR | <13.8 | 88.5–116 | [56] |
| WTP | NDMA, NMEA, NPyr, NDEA, NPip, NMor, NDPA, NDBA, NDPhA, NNN, NAT, NAB, NNK, NNAL | SPE Oasis HLB cartridge/SPE absorbents LiChrolut EN (vinyl/divinyl polymer) and Ambersorb 572 (activated carbon) Sigma-Aldrich. |
HPLC (Agilent 1100) |
Kinetex C8 column (100 × 3.0 mm i.d., 2.6 μm; Phenomenex) | MS/MS | 0.01–2.7 ng/L | 0.03–8.8 ng/L | NR | 53–93 | [21] |
| Drinking Water | d6-NDMA, NDMA, NMEA, NDEA, NDPA, NPYR NMOR, NPIP, NDBA, NDPhA | SPE (CCC) (CNW Technologies) USEPA Method 521 | GC Agilent 6890 N |
DB-35MS was used (35% diphenyl/65% dimethyl polysiloxane) | Agilent QMSS 5975 |
NR | 1.5–4.9 ng/L | NR | 65–122 | [18] |
| Drinking Water | NMEA, NDEA, NDMA, NDPA, NPyr, NPip, NDBA, NDMA-d6 | SPME (57330-U, Supelco) | GC Agilent 7890 | Agilent DB-624 column (30 m_ 0.25 mm I. D. 1.4 mm) |
Agilent MS 5975. | 0.12–0.79 ng/L), | 0.1–0.8 ng/L | <10 | 77–114 | [57] |
| Finished/tap/source water | NDMA, NDEA, NMOR, NPIP, NDBA |
SPE (CCC) (Auto Trace 280, Dionex, Corp) CNW Technologie) EPA 521 method | UPLC (Agilent 1100) | A C8 (2) Capillary column (150 × 0.32 mm i.d., 5 ím) |
MS/MS (API 4000 QTrap Applied Biosystems/MDS Sciex) | 0.1–1 ng/L | NR | 1.4–5.1 | 64–116 | [16] |
| Wastewater | NDMA, NMEA, NDEA, NDBA, NPIP, NPYR, NMOR, THEOB, XAN, THEOP | SPE Strata-X polymeric (100 mg/6 mL) Phenomenex/SPE (CCC) (200 mg/6 mL), Supelco | GC | 30 m × 0.25 mm i.d. × 0.25 _m SLB-IL111 (Supelco). | MS/MS A Brucker 320-MS. |
<30.6 ng/L | <48.6 ng/L | <10 | NR | [58] |
| Drinking/MilliQ water | NDMA Nmor Npyr NMEA NDEA Npip NDPA NDBA NDPhA | SPE | UPLC (Acquity HSS T3) | 50 mm × 2.1 mm, × 1.8 μm particle size. | MS Waters (Micromass Quattro Premier XE) |
<0.9 ng/L | NR | NR | 70–90 | [2] |
| Potable Water |
NDMA, NDMA-d6 Toluene-d8 |
SPE (Sep-Pak AC-2 cartridge) | GC Varian 450 |
30 m × 0.25 mm × 1.0 lm | MS Varian 300 |
<2 ng/L | NR | <11.1 | 70–120 | [59] |
| Drinking Water | NMEA, NDPA, NDEA, NDBA, NMor, NPip, NPyr. |
LLE (with dichloromethane) | GC Agilent 6890 | 40 × 0.18 mm ID and 1 μm (RTX-VMS) | MS Agilent 5973 |
0.4–2.0 ng/L | 10 ng/L | <19 | 95 | [60] |
| Sewage | NDMA, NMOR, NPYR | SPE | HPLC Agilent HP1100 /GC QP2010 Shimadzu |
NR | MS/MS (Acquity TQD) | NR | 5.0–25 ng/L /1.0 ng/L |
NR | NR | [61] |
| Bio solid | NDMA, NMEA, NDPA NDBA NPYR, NPIP, NDPhA | LLE (2 mL dichloromethane per g of biosolids) | HPLC (Shimadzu) | 130 Å, 3.5 μm, 4.6 × 150 mm. | MS/MS API 4000 (Applied Biosystems) |
0.06–5.7 ng/g | NR | NR | 90–126 | [62] |
| Meat Products (Pork Sausage) | NDMA, NMEA, NDEA, NPYR, NDPA, NPIP, NDBA | D-l-SPE | GC Varian 450 | 30 m × 0.25 mm × 1.0 l, DB5-MS. | MS (Varian 2200 | 0.01–0.12 (ng/g) | 0.03–0.36 (ng/g) | <10 | 74–105 | [51] |
| Deionized Water Water |
NDMA, DMTA | SPME (PDMS/DVB, 65 μm, Supelco) | GC Thermo TRACE. | 30 m × 0.25 mm 0.25 μm, (ZB-5ms Zebron, Phenomenex). |
MS (Thermo TRACE DSQ II). | 0.3–0.6 μM |
2.5–16 Μm | 0.2–0.8 | NR | [63] |
| Cosmetic | NDMA, NMEA, NDEA, NPYR, NDPA, NPIP, NDBA | HS-SPME (splitless liner 0.75 mm i.d. Agilent) | GC Agilent 7890B |
30 mm × 0.25 μm I.D × 0.25 μm, DB-WAX Agilent (Palo Alto) | MS Agilent 7693 |
0.46–36.54 ng/g | NR | <20 | 79 | [8] |
N-nitrosonornicotine NNN, N-nitrosoanatabine NAT N-nitrosoanabasine NAB, 4-(methylnitrosamino)-1-(3-pyridyl)-1-butanone NNK, 4-(methylnitrosamino)-1-(3-pyridyl)-1-butanol NNAL, Caffeine CAF; Theophylline THEOP, 1,7-dimethylxanthine XAN, Theobromine THEOB. Coconut charcoal cartridge (CCC). Not Registered (NR), Solid Phase Extraction (SPE), Secondary (2o), Effluent (E), Solid-phase micro extraction (SPME), high-performance liquid chromatography (HPLC), ultra-fast liquid chromatography–tandem mass spectrometry(UFLC-MS/MS), Trap mass spectrometer (TMS), Dimethylamine (DMA),Ethylmethylamine (EMA), Diethylamine (DEA), Dipropylamine (DPA), Trimethylamine (TMA), 3-(Dimethylaminomethyl)indole (DMAI), 4-Dimethylami- noantipyrine (DMAP), Electrospray Ionization (ESI), Tandem Quad (TQD) MS Technology, Water treatment plant (WTP). Qudrupole mass selective spectrometer (QMSS), (NDMA: N-nitrosodimethylamine, International Sorbent Technology (IST), Temperature: temp. Dispersive micro solid-phase extraction (D-l-SPE), Deuterated toluene (toluene-d8), Liquid-liquid extraction (LLE), Head space solid-phase micro extraction (HS-SPME).