使用 Anyeep TQ9100测定水质中53种全氟化合物的方法 - 技术应用

Studies show that per- and polyfluoroalkyl substances (PFAS) are persistent and bioaccumulative, accumulating in organisms at levels hundreds to thousands of times higher than known persistent organic pollutants such as organochlorine pesticides and dioxins. PFAS also exhibit reproductive toxicity, mutagenicity, developmental toxicity, neurotoxicity, and immunotoxicity, making them a class of environmental contaminants with systemic multi-organ toxicity. Observed toxic effects in toxicological studies include: immune system suppression, impaired mitochondrial metabolism, liver cell damage, reproductive cell injury, reduced fertility and reproductive capacity, adverse effects on late-stage fetal development, alterations in gene expression, and interference with enzyme activity.

Routine testing covers animal- and plant-derived foods, feed, water quality, and other matrices. Applicable standards include GB/T 5750.8-2023, SN/T 4588-2016, SN/T 5222-2019, DB35/T 1693-2017, and DB32/T 4004-2021. This method is based on GB/T 5750.8-2023 §84, with the analyte list expanded to 15 perfluorinated compounds and their derivatives, quantified using the internal standard method.

Instruments and Reagents

Anyeep TQ9100 Ultra-High Performance Liquid Chromatography-Tandem Mass Spectrometry System

Acetonitrile (Mass Spectrometry Grade, Thermo Fisher Scientific, USA)

Water (Ultra-pure Water)

Ammonium Acetate (Merck KGaA, Germany)

Anion Exchange Solid Phase Extraction Cartridge（Shanghai Anpel, SBEQ-CA3881）

Liquid Chromatography Conditions

Mobile Phase A：Water, containing 2 mM ammonium acetate

Mobile Phase B： Acetonitrile

Chromatography column： Agilent ZORBAX Eclipse Plus C18 2.1×100 mm 1.8µm

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： 7

Scan Mode: MRM

Gradient elution program

Time (min)	A %	B %	Flow Rate mL/min
0.0	85	15	0.3
2.0	55	45	0.3
12.0	10	90	0.3
16.0	10	90	0.3
16.1	85	15	0.3
20.0	85	15	0.3

Analyte MRM Parameters

No.	Test Item	Q1 Ion	Q3 Ion	Residency Time (ms)	CE (V)	DP (V)
1	PFBA	213	169*	20	1	40
2	PFMPA	229	85*	20	13	25
		229	185	20	4	25
3	3:3 FTCA	241	177	20	20	30
		241	117*	20	40	30
4	PFPeA	263	219*	20	1	30
		263	69	20	53	30
5	PFBS	299	80*	20	55	70
		299	99	20	58	70
6	PFMBA	279	85*	20	3	25
		279	235	20	4	25
7	PFEESA	315	135*	20	5	30
		315	69	20	48	30
8	NFDHA	201	85*	20	25	25
		295	201	20	1	25
9	4:2 FTS	327	307*	20	19	50
		327	81	20	42	50
10	PFHxA	313	269*	20	8	15
		313	119	20	21	15
11	PFPeS	349	80*	20	70	60
		349	99	20	50	60
12	HFPO-DA	285	169*	20	2	50
		285	185	20	17	50
13	FBSA	298	78	20	35	80
		298	119*	20	15	80
14	PFHpA	363	319*	20	10	35
		363	169	20	11	35
15	PFHxS	399	80*	20	75	150
		399	99	20	75	85
16	5:3 FTCA	341	237*	20	10	60
		341	217	20	5	60
17	6:2 FTUCA	357	293*	20	35	10
		357	243	20	40	10
18	ADONA	377	251*	20	20	50
		377	85	20	29	50
19	6:2 FTCA	377	293*	20	15	40
		377	63	20	35	40
20	6:2 Full-Text Search	427	407*	20	24	20
		427	81	20	47	40
21	PFOA	413	369	20	15	35
		413	169*	20	15	35
22	PFHpS	449	80*	20	82	80
		449	99	20	76	85
23	PFOS	499	80	20	85	80
		499	99*	20	95	60
24	FHxSA	398	78*	20	61	40
		398	169	20	31	150
25	PFNA	463	419*	20	14	40
		463	219	20	13	40
26	8:2 FTUCA	457	393*	20	40	30
		457	243	20	40	30
27	7:3 FTCA	441	337*	20	20	50
		441	317	20	50	50
28	8:2 FTCA	477	393*	20	12	30
		477	63	20	30	30
29	HFPO-TA	495	119*	20	50	50
		495	185	20	20	50
30	9Cl-PF3ONS	531	351*	20	15	50
		531	83	20	31	85
31	FDA	513	469*	20	12	60
		513	219	20	14	60
32	PFNS	549	80*	20	95	100
		549	99	20	100	80
33	8:2 Full-Text Search	527	507*	20	27	50
		527	81	20	74	50
34	NMeFOSAA	570	419*	20	10	40
		570	483	20	5	40
35	OBS	603	172*	20	40	40
		603	465	20	15	60
36	PFDS	599	80*	20	95	85
		599	99	20	95	80
37	NEtFOSAA	584	419*	50	17	40
		584	526	50	25	40
38	PFUnDA	563	519	20	15	60
		563	269*	20	21	60
39	10:2 FTCA	577	493*	20	25	40
		577	63	20	50	40
40	11Cl-PF3OUdS	631	451*	20	20	85
		631	83	20	69	50
41	10:2 FTUCA	557	493*	20	20	50
		557	119	20	50	30
42	FOSA	498	78*	20	25	30
		498	169	20	30	30
43	PFUnDS	649	80*	20	105	100
		649	99	20	105	60
44	PFDoA	613	569*	20	6	60
		613	269	20	21	60
45	PFDoDS	699	80*	20	105	80
		699	99	20	90	80
46	PFTrDA	663	619*	20	9	60
		663	269	20	25	60
47	6:2 diPAP	789	97	20	80	60
		789	443*	20	20	80
48	PFTeDA	713	669*	20	17	60
		713	369	20	25	60
49	NMeFOSA	512	219*	20	24	110
		512	169	20	28	110
50	NEtFOSA	526	219*	50	26	110
		526	169	50	28	110
51	PFHxDA	813	769*	20	8	70
		813	369	20	25	70
52	8:2 diPAP	989	97*	20	100	100
		989	543	20	29	100
53	PFODA	913	869*	20	17	120
		913	369	20	30	120

Sample Processing

Measure 500 ml of water sample, add 50.0 µl of extraction internal standard, mix well, filter through membrane, and adjust the pH of the filtered water sample to 6–7 using acetic acid or ammonia.

Add the above water sample to a pre-activated weak anion exchange solid-phase extraction (SPE) cartridge. Pass it through the cartridge at a flow rate of 3 ml/min–5 ml/min. Rinse the cartridge sequentially with 6 ml of water and 8 ml of ammonium acetate buffer; discard the rinse eluates. Dry the cartridge under vacuum, then elute sequentially with 8 ml of methanol and 6 ml of ammonia-methanol solution at a flow rate of 1 ml/min–3 ml/min. Combine both eluates, evaporate to near dryness using nitrogen, add 50.0 µl of internal standard for injection, and dilute to volume with methanol to 1.0 ml. Mix well, filter through a syringe filter, and proceed for analysis.。

Summary
This document establishesUseUltra-High-Performance Liquid Chromatography-Tandem Mass Spectrometry System Anyeep TQ9100 analyzes 53 perfluorinated compounds. The results demonstrate excellent sensitivity, stability, and linear range, making it suitable for routine water quality analysis of perfluorinated compounds.

Method for Determining 53 Perfluorinated Compounds in Water Using Anyeep TQ9100