Method for Determining 17 Perfluorinated Compounds in Drinking Water Using Anyeep TQ9120
This study established a method for detecting 17 per- and polyfluoroalkyl substances (PFAS) in drinking water using Anyeep TQ9120, an ultra-high-performance liquid chromatography-tandem mass spectrometry system from Anyeep. The method demonstrates excellent linearity, with detection limits and quantification limits meeting relevant regulatory standards. Using this method and equipment enables the identification and quantification of 17 PFAS compounds.
Perfluorinated compounds are persistent and bioaccumulative.，Accumulation levels are hundreds to thousands of times higher than those of known organochlorine pesticides and dioxins.。Per- and polyfluoroalkyl substances (PFAS) exhibit reproductive, mutagenic, developmental, neurotoxic, and immunotoxic effects. They are environmental pollutants that cause systemic toxicity across multiple organs.The "GB 5749-2022 Standard for Drinking Water Hygiene" explicitly sets detection limits for perfluorooctanoic acid (PFOA), perfluorooctane sulfonic acid (PFOS), and related substances in drinking water.
This method was developed to simultaneously detect 17 perfluorinated compounds in drinking water, based on the requirements for perfluorooctanoic acid (PFOA) testing outlined in Section 84 of "GB/T 5750.8-2023 Methods for Examination of Drinking Water - Part 8: Organic Indicators."
Instruments and Reagents
Anyeep TQ120 Ultra-High Performance Liquid Chromatography-Tandem Mass Spectrometry System
Methanol (mass spectrometry grade, Thermo Fisher Scientific, USA)
Acetic acid, ammonium acetate（ChromatographyPureGermany's Merk Company）
AmmoniaWater (Analytical Grade, Shanghai Anpel）
17-component Perfluorinated Compound Mixture Standard(Shanghai ANPEL, 81589x）
3-component Perfluorinated Compound Internal Standard Mixture (Shanghai ANPEL, 83216x)
Anion Exchange Solid Phase Extraction Cartridge（Shanghai Anpel, SBEQ-CA3881）
Liquid Chromatography Conditions
Mobile Phase A：Water, containing 5 mM ammonium acetate
Mobile Phase B： Methanol
Chromatography column： WatersAcquity UPLCBEH C18，1.7 µm， 2.1 × 100 mm
stream Fast： 0.3mL/min
Column Warm： 40 ℃
Injection volume：5μL
Mass Spectrometry Conditions
Ionization Source： Electrospray Ionization Source (ESI)-）
Source Warm degree： 550 ℃
Spray Voltage： -4500 V
Qi curtain Qi： 30 psi
Fog Qi： 60psi
Assist Help Qi： 60psi
Clap Crash Qi： 11
Scan Mode：MRM
Gradient elution program
Time (min) | A % | B % | Flow Rate mL/min |
0.0 | 80 | 20 | 0.3 |
1.5 | 60 | 40 | 0.3 |
10.0 | 10 | 90 | 0.3 |
10.1 | 2 | 98 | 0.3 |
12.0 | 2 | 98 | 0.3 |
12.1 | 80 | 20 | 0.3 |
14.0 | 80 | 20 | 0.3 |
Analyte MRM Parameters
Test Item | Q1 Ion | Q3 Ion | CE(V) | DP(V) |
PFBA Perfluorobutyric acid | 212 | 169 | 2 | 30 |
212 | 97 | 2 | 30 | |
PFPeA Perfluoropentanoic acid | 263 | 219 | 45 | 30 |
263 | 69 | 4 | 30 | |
PFHxA Perfluorohexanoic acid | 313 | 269 | 15 | 30 |
313 | 119 | 4 | 30 | |
PFHpA Perfluoroheptanoic acid | 363 | 319 | 14 | 30 |
363 | 169 | 2 | 30 | |
PFOA Perfluorooctanoic acid | 413 | 369 | 12 | 30 |
413 | 169 | 2 | 30 | |
PFNA Perfluorononanoic acid | 463 | 419 | 14 | 30 |
463 | 169 | 2 | 30 | |
FDA Perfluorodecanoic acid | 513 | 469 | 14 | 30 |
513 | 219 | 5 | 30 | |
PFUnDA Perfluoroundecanoic acid | 563 | 519 | 15 | 60 |
563 | 319 | 6 | 60 | |
PFDoDA Perfluorododecanoic acid | 613 | 569 | 20 | 60 |
613 | 169 | 6 | 60 | |
PFTrDA Perfluorotridecanoic acid | 663 | 619 | 22 | 60 |
663 | 169 | 6 | 60 | |
PFTeDA Perfluorotetradecanoic acid | 713 | 669 | 24 | 90 |
713 | 169 | 10 | 90 | |
PFHxDA Perfluorohexadecanoic acid | 813 | 769 | 28 | 120 |
813 | 169 | 12 | 120 | |
PFODA Perfluorooctanoic acid | 913 | 869 | 38 | 120 |
913 | 169 | 58 | 120 | |
PFBS Perfluorobutane sulfonate | 299 | 80 | 56 | 90 |
299 | 99 | 68 | 90 | |
PFHxS Perfluorohexanesulfonic acid | 399 | 80 | 68 | 120 |
399 | 99 | 70 | 120 | |
PFOS Perfluorooctane sulfonic acid | 499 | 80 | 68 | 150 |
499 | 99 | 80 | 150 | |
PFDS Perfluorodecanesulfonic acid | 599 | 80 | 80 | 180 |
599 | 99 | 2 | 180 | |
PFHxA-13C2 | 315 | 270 | 15 | 30 |
PFOA-13C4 | 417 | 372 | 12 | 30 |
PFOS-13C4 | 503 | 80 | 68 | 150 |
Sample Processing
Measure 1 L Test Water Sample，Add 4.625 g ammonium acetate, acetic acidAdjustpHTo 6.8 - 7.0，Add per liter of water sample100 mcg Isotope Internal Standard Mixture Solution 100 μL，Mix，0.22 μmCellulose acetate membraneFilter
Extract using pre-activated weak anion exchange solid-phase extraction (SPE) cartridges, sequentially with 0.1% mass fractionAmmonia-methanol solution5 mL, Methanol7 mLand pure water10 mLActivate), control the flow rate at approximately 8 mL/min. Rinse with 25 mM ammonium acetate solution (pH adjusted to 4.0 using acetic acid) 5 mL and deionized water 12 mL, then dry under vacuum for 15 min. Proceed sequentially with:Methanol5 mLammonia-methanol solution7 mLPerform elution，Collect all eluates。40 ℃Evaporate to dryness under nitrogen stream. Reconstitute with 1 mL of methanol-water solution (methanol:water 3:7, v/v). 5μL injection.
Linear Range
Test Item | Retention Time min | Limit of Detection μg/L | Method detection limit ng/L | Linear Range μg/L | Linear Equation 1/x2 | correlation coefficient r2 |
PFBA | 2.31 | 0.2 | 0.2 | 0.5-200 | y = 194.496 * x + 73.7965 | 0.9935 |
PFPeA | 3.96 | 0.2 | 0.2 | 0.5-200 | y = 1125.76 * x + 15.1260 | 0.9991 |
PFBS | 4.39 | 0.01 | 0.01 | 0.02-200 | y = 596.905 * x + 1.52550 | 0.9950 |
PFHxA | 5.43 | 0.02 | 0.02 | 0.1-200 | y = 1473.82 * x + 6.25335 | 0.9976 |
PFHpA | 6.59 | 0.02 | 0.02 | 0.1-200 | y = 1649.93 * x + 8.86020 | 0.9978 |
PFHxS | 6.70 | <0.01 | <0.01 | 0.01-200 | y = 463.553 * x + 0.59411 | 0.9952 |
PFOA | 7.48 | 0.2 | 0.2 | 0.5-200 | y = 1920.98 * x + 4.80332 | 0.9979 |
PFNA | 8.26 | 0.02 | 0.02 | 0.1-200 | y = 2106.58 * x + 23.5707 | 0.9959 |
PFOS | 8.28 | 0.01 | 0.01 | 0.02-200 | y = 380.290 * x + 1.39007 | 0.9944 |
FDA | 8.89 | 0.02 | 0.02 | 0.1-200 | y = 317.343 * x + 1.99813 | 0.9941 |
PFDS | 9.44 | 0.01 | 0.01 | 0.02-200 | y = 270.518 * x + 0.35341 | 0.9930 |
PFUnDA | 9.45 | 0.02 | 0.02 | 0.1-200 | y = 2243.58 * x + 15.3498 | 0.9911 |
PFDoDA | 9.91 | 0.02 | 0.02 | 0.1-200 | y = 109.115 * x + 0.06470 | 0.9953 |
PFTrDA | 10.31 | 0.02 | 0.02 | 0.1-200 | y = 89.6985 * x + 0.51377 | 0.9908 |
PFTeDA | 10.64 | 0.1 | 0.1 | 0.2-200 | y = 1547.08 * x + 21.4153 | 0.9912 |
PFHxDA | 11.19 | 0.2 | 0.2 | 0.5-200 | y = 450.902 * x + 21.1795 | 0.9979 |
PFODA | 11.61 | 0.2 | 0.2 | 0.5-200 | y = 109.504 * x + 14.6840 | 0.9935 |
Accuracy and Precision
Test Item | Add label ng/L | background ng/L | 1 | 2 | 3 | 4 | 5 | Precision | Recovery Rate |
PFBA | 2 | 0 | 2.22 | 2.14 | 2.23 | 2.08 | 2.04 | 3.91% | 107.1% |
| 10 | 0 | 9.76 | 9.21 | 9.39 | 9.43 | 10.14 | 3.84% | 95.9% |
PFPeA | 1 | 0 | 1.13 | 1.1 | 1.1 | 1.06 | 1.14 | 2.83% | 110.6% |
| 10 | 0 | 9.62 | 9.39 | 9.36 | 9.15 | 9.59 | 2.03% | 94.2% |
PFBS | 1 | 0 | 1.14 | 1.04 | 1.12 | 1.05 | 1.08 | 3.99% | 108.6% |
| 10 | 0 | 10.11 | 9.8 | 9.67 | 9.61 | 9.95 | 2.08% | 98.3% |
PFHxA | 1 | 0 | 1.14 | 1.07 | 1.06 | 1.07 | 1.08 | 2.96% | 108.4% |
| 10 | 0 | 10.13 | 9.97 | 9.78 | 9.52 | 9.92 | 2.33% | 98.6% |
PFHpA | 1 | 0 | 1.08 | 1.02 | 1.05 | 1.07 | 1.03 | 2.43% | 105.0% |
| 10 | 0 | 9.43 | 9.59 | 9.58 | 9.37 | 9.46 | 1.01% | 94.9% |
PFHxS | 1 | 0 | 1.15 | 1.11 | 1.09 | 1.1 | 1.05 | 3.28% | 110.0% |
| 10 | 0 | 10.28 | 9.93 | 9.97 | 9.53 | 9.71 | 2.87% | 98.8% |
PFOA | 1 | 0 | 1.11 | 0.96 | 0.98 | 1.06 | 1.05 | 5.95% | 103.2% |
| 10 | 0 | 10.62 | 9.95 | 9.94 | 9.24 | 9.76 | 4.99% | 99.0% |
PFNA | 1 | 0 | 1.15 | 1.07 | 1.1 | 1.14 | 1.19 | 4.10% | 113.0% |
| 10 | 0 | 10.11 | 10.17 | 10.08 | 9.43 | 9.7 | 3.24% | 99.0% |
PFOS | 1 | 0 | 1.09 | 1.02 | 1.04 | 1.08 | 0.95 | 5.40% | 103.6% |
| 10 | 0 | 9.65 | 10 | 9.73 | 9.51 | 8.89 | 4.32% | 95.6% |
FDA | 1 | 0 | 1.13 | 1.04 | 1.04 | 1.1 | 1.1 | 3.72% | 108.2% |
| 10 | 0 | 9.21 | 9.69 | 9.49 | 8.94 | 8.8 | 4.01% | 92.3% |
PFDS | 1 | 0 | 1.17 | 1.18 | 1.18 | 1.17 | 1.12 | 2.16% | 116.4% |
| 10 | 0 | 9.6 | 10.07 | 10.01 | 9.65 | 9.13 | 3.90% | 96.9% |
PFUnDA | 1 | 0 | 1.15 | 1.11 | 1.14 | 1.13 | 1.14 | 1.34% | 113.4% |
| 10 | 0 | 9.85 | 10.2 | 10.27 | 9.91 | 8.98 | 5.23% | 98.4% |
PFDoDA | 1 | 0 | 1.16 | 1.14 | 1.1 | 1.1 | 1.21 | 4.03% | 114.2% |
| 10 | 0 | 10.52 | 10.31 | 9.74 | 9.63 | 9.46 | 4.61% | 99.3% |
PFTrDA | 1 | 0 | 1.12 | 1.13 | 1.04 | 1.13 | 1.14 | 3.67% | 111.2% |
| 10 | 0 | 8.57 | 8.36 | 8.74 | 8.19 | 7.53 | 5.64% | 82.8% |
PFTeDA | 1 | 0 | 1.16 | 1.16 | 1.11 | 1.16 | 1.17 | 2.07% | 115.2% |
| 10 | 0 | 9.01 | 9.26 | 8.94 | 9.2 | 8.68 | 2.55% | 90.2% |
PFHxDA | 1 | 0 | 1.13 | 1.12 | 1.16 | 1.15 | 1.18 | 2.08% | 114.8% |
| 10 | 0 | 7.74 | 8.61 | 8.38 | 8.54 | 8.01 | 4.48% | 82.6% |
PFODA | 1 | 0 | 1.03 | 0.97 | 1.11 | 1.02 | 1.19 | 8.13% | 106.4% |
| 10 | 0 | 7.69 | 8.92 | 8.15 | 8.75 | 8.06 | 6.13% | 83.1% |
Summary
This study established an ultra-high-performance liquid chromatography-tandem mass spectrometry system (Anyeep TQ91).20 AnalysisPotable Waterzh17 perfluorinated compoundsdetection method. As shown in the results, this method exhibits excellent sensitivity, stability, and a wide linear range.Recovery rate meets national standard requirements.Suitable forPer- and polyfluoroalkyl substances in drinking waterRoutine analysis and testing.