色谱 ›› 2024, Vol. 42 ›› Issue (11): 1032-1041.DOI: 10.3724/SP.J.1123.2024.02010
邱巧丽, 潘胜东, 王立, 方兰云, 陈晓红, 金米聪*()
收稿日期:
2024-02-18
出版日期:
2024-11-08
发布日期:
2024-10-22
通讯作者:
* E-mail:基金资助:
QIU Qiaoli, PAN Shengdong, WANG Li, FANG Lanyun, CHEN Xiaohong, JIN Micong*()
Received:
2024-02-18
Online:
2024-11-08
Published:
2024-10-22
Supported by:
摘要:
建立了基于EMR-Lipid的分散固相萃取-超高效液相色谱-三重四极杆质谱法(UPLC-MS/MS)同时快速准确测定牛肉中17种全氟烷基化合物(perfluoroalkyl substances, PFASs)残留的检测方法。样品经含0.1%(v/v)甲酸的乙腈溶液提取后,采用100 mg PSA+80 mg C18+40 mg GCB+150 mg EMR-Lipid混合填料进行分散固相萃取净化,采用0.5 mmol/L氟化铵水溶液-甲醇体系为流动相,在Acquity Premier BEH C18色谱柱(100 mm×2.1 mm, 1.7 μm)上进行梯度洗脱分离,流速为0.3 mL/min,采用电喷雾负离子多反应监测(MRM)模式进行检测,内标法定量分析。在最佳的实验条件下,17种PFASs的线性范围为0.2~20.0 μg/L,相关系数为0.9915~0.9999。方法检出限为0.003~0.007 μg/kg,方法定量限为0.01~0.02 μg/kg。在0.05、0.5、1.8 μg/kg 3个加标水平下,17种PFASs的加标回收率为71.1%~127.4%, RSD为0.6%~14.4%。研究结果还表明:在本研究优化的色谱条件下,相比于不同浓度(2.0、5.0、10.0 mmol/L)的甲酸铵或乙酸铵水溶液-甲醇体系,0.5 mmol/L氟化铵水溶液-甲醇体系作为流动相时,17种PFASs的灵敏度均有提高,其中羧酸类长链PFASs(C10~C18)的灵敏度可提高1~2倍。相比于单独使用PSA、C18、GCB、EMR-Lipid吸附材料和PSA+C18+GCB组合吸附材料,本文选择的PSA+C18+GCB+EMR-Lipid混合吸附材料具有对油脂基质去除效果更佳的特点。该方法操作简便快速,灵敏度高,基质效应低,重复性好,可用于牛肉中多种全氟烷基化合物的同时快速准确检测。
中图分类号:
邱巧丽, 潘胜东, 王立, 方兰云, 陈晓红, 金米聪. 基于EMR-Lipid分散固相萃取-超高效液相色谱-串联质谱法同时测定牛肉中17种全氟烷基化合物[J]. 色谱, 2024, 42(11): 1032-1041.
QIU Qiaoli, PAN Shengdong, WANG Li, FANG Lanyun, CHEN Xiaohong, JIN Micong. Simultaneous determination of 17 perfluoroalkyl substances in beef by EMR-Lipid dispersive solid-phase extraction and ultra performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Chromatography, 2024, 42(11): 1032-1041.
Compound | tR/ min | Precursor ion (m/z) | Product ion (m/z) | Declustering potential/V | Collision energy/eV | IS |
---|---|---|---|---|---|---|
Perfluorobutanoic acid (PFBA) | 2.42 | 213.0 | 168.9* | -19 | -13 | PFBA-13C4 |
Perfluoropentanoic acid (PFPeA) | 3.19 | 263.0 | 218.9* | -26 | -11 | PFBA-13C4 |
Perfluorobutanesulfonic acid (PFBS) | 3.29 | 298.9 | 80.0* | -70 | -65 | PFOS-13C4 |
99.0 | -70 | -36 | ||||
Perfluorohexanoic acid (PFHxA) | 3.62 | 312.9 | 268.9* | -11 | -11 | PFHxA-13C2 |
119.0 | -11 | -26 | ||||
Perfluoroheptanoic acid (PFHpA) | 4.08 | 362.9 | 318.9* | -20 | -14 | PFHxA-13C2 |
168.9 | -20 | -24 | ||||
Perfluorohexanesulfonic acid (PFHxS) | 4.12 | 398.9 | 80.0* | -70 | -75 | PFHxS-18O2 |
99.0 | -70 | -79 | ||||
Perfluorooctanoic acid (PFOA) | 4.70 | 412.9 | 368.9* | -30 | -15 | PFOA-13C4 |
168.9 | -30 | -25 | ||||
Perfluorononanoic acid (PFNA) | 5.39 | 462.9 | 418.9* | -19 | -14 | PFNA-13C5 |
218.9 | -19 | -23 | ||||
Perfluorooctanesulfonic acid (PFOS) | 5.43 | 498.9 | 80.0* | -60 | -96 | PFOS-13C4 |
99.0 | -60 | -99 | ||||
Perfluorodecanoic acid (PFDA) | 6.09 | 512.9 | 468.9* | -33 | -16 | PFDA-13C2 |
218.9 | -33 | -24 | ||||
Perfluoroundecanoic acid (PFUnDA) | 6.73 | 562.9 | 518.9* | -29 | -19 | PFUnDA-13C2 |
268.9 | -29 | -26 | ||||
Perfluorodecanesulfonic acid sodium (PFDS) | 6.73 | 598.8 | 79.9* | -100 | -100 | PFOS-13C4 |
98.9 | -100 | -100 | ||||
Perfluorododecanoic acid (PFDoDA) | 7.32 | 612.8 | 569.0* | -20 | -19 | PFDoDA-13C2 |
168.9 | -20 | -33 | ||||
Perfluorotridecanoic acid (PFTrDA) | 7.84 | 662.8 | 618.8* | -40 | -17 | PFDoDA-13C2 |
168.9 | -40 | -34 | ||||
Perfluorotetradecanoic acid (PFTeDA) | 8.27 | 712.8 | 668.8* | -40 | -17 | PFDoDA-13C2 |
168.9 | -40 | -39 | ||||
Perfluorohexadecanoic acid (PFHxDA) | 9.01 | 812.9 | 768.9* | -30 | -22 | PFDoDA-13C2 |
168.9 | -30 | -35 | ||||
Perfluorooctadecanoic acid (PFODA) | 9.58 | 912.9 | 868.9* | -30 | -22 | PFDoDA-13C2 |
218.9 | -30 | -35 | ||||
Perfluoro-n-[13C4]butanoic acid (PFBA-13C4) | 2.42 | 216.9 | 171.9* | -19 | -13 | |
Perfluoro-n-[1,2-13C2]hexanoic acid (PFHxA-13C2) | 3.61 | 314.9 | 269.9* | -11 | -11 | |
Perfluoro-n-[1,2,3,4-13C4]octanoic acid (PFOA-13C4) | 4.70 | 416.9 | 372.0* | -30 | -15 | |
Perfluoro-n-[1,2,3,4,5-13C5]nonanoic acid (PFNA-13C5) | 5.39 | 467.9 | 422.9* | -19 | -14 | |
Perfluoro-n-[1,2-13C2]decanoic acid (PFDA-13C2) | 6.08 | 514.9 | 469.9* | -33 | -24 | |
Perfluoro-n-[1,2-13C2]undecanoic acid (PFUnDA-13C2) | 6.73 | 564.9 | 519.9* | -29 | -15 | |
Perfluoro-n-[1,2-13C2]dodecanoic acid (PFDoDA-13C2) | 7.32 | 614.8 | 569.9* | -20 | -19 | |
Sodium perfluoro-1-hexane[18O2]sulfonate (PFHxS-18O2) | 4.12 | 402.9 | 83.9* | -70 | -75 | |
Sodium perfluoro-1-[1,2,3,4-13C4]octanesulfonate (PFOS-13C4) | 5.42 | 502.9 | 79.9* | -60 | -96 |
表1 17种PFASs及9种内标的质谱参数
Table 1 MS parameters of the 17 perfluoroalkyl substances (PFASs) and 9 internal standards (ISs)
Compound | tR/ min | Precursor ion (m/z) | Product ion (m/z) | Declustering potential/V | Collision energy/eV | IS |
---|---|---|---|---|---|---|
Perfluorobutanoic acid (PFBA) | 2.42 | 213.0 | 168.9* | -19 | -13 | PFBA-13C4 |
Perfluoropentanoic acid (PFPeA) | 3.19 | 263.0 | 218.9* | -26 | -11 | PFBA-13C4 |
Perfluorobutanesulfonic acid (PFBS) | 3.29 | 298.9 | 80.0* | -70 | -65 | PFOS-13C4 |
99.0 | -70 | -36 | ||||
Perfluorohexanoic acid (PFHxA) | 3.62 | 312.9 | 268.9* | -11 | -11 | PFHxA-13C2 |
119.0 | -11 | -26 | ||||
Perfluoroheptanoic acid (PFHpA) | 4.08 | 362.9 | 318.9* | -20 | -14 | PFHxA-13C2 |
168.9 | -20 | -24 | ||||
Perfluorohexanesulfonic acid (PFHxS) | 4.12 | 398.9 | 80.0* | -70 | -75 | PFHxS-18O2 |
99.0 | -70 | -79 | ||||
Perfluorooctanoic acid (PFOA) | 4.70 | 412.9 | 368.9* | -30 | -15 | PFOA-13C4 |
168.9 | -30 | -25 | ||||
Perfluorononanoic acid (PFNA) | 5.39 | 462.9 | 418.9* | -19 | -14 | PFNA-13C5 |
218.9 | -19 | -23 | ||||
Perfluorooctanesulfonic acid (PFOS) | 5.43 | 498.9 | 80.0* | -60 | -96 | PFOS-13C4 |
99.0 | -60 | -99 | ||||
Perfluorodecanoic acid (PFDA) | 6.09 | 512.9 | 468.9* | -33 | -16 | PFDA-13C2 |
218.9 | -33 | -24 | ||||
Perfluoroundecanoic acid (PFUnDA) | 6.73 | 562.9 | 518.9* | -29 | -19 | PFUnDA-13C2 |
268.9 | -29 | -26 | ||||
Perfluorodecanesulfonic acid sodium (PFDS) | 6.73 | 598.8 | 79.9* | -100 | -100 | PFOS-13C4 |
98.9 | -100 | -100 | ||||
Perfluorododecanoic acid (PFDoDA) | 7.32 | 612.8 | 569.0* | -20 | -19 | PFDoDA-13C2 |
168.9 | -20 | -33 | ||||
Perfluorotridecanoic acid (PFTrDA) | 7.84 | 662.8 | 618.8* | -40 | -17 | PFDoDA-13C2 |
168.9 | -40 | -34 | ||||
Perfluorotetradecanoic acid (PFTeDA) | 8.27 | 712.8 | 668.8* | -40 | -17 | PFDoDA-13C2 |
168.9 | -40 | -39 | ||||
Perfluorohexadecanoic acid (PFHxDA) | 9.01 | 812.9 | 768.9* | -30 | -22 | PFDoDA-13C2 |
168.9 | -30 | -35 | ||||
Perfluorooctadecanoic acid (PFODA) | 9.58 | 912.9 | 868.9* | -30 | -22 | PFDoDA-13C2 |
218.9 | -30 | -35 | ||||
Perfluoro-n-[13C4]butanoic acid (PFBA-13C4) | 2.42 | 216.9 | 171.9* | -19 | -13 | |
Perfluoro-n-[1,2-13C2]hexanoic acid (PFHxA-13C2) | 3.61 | 314.9 | 269.9* | -11 | -11 | |
Perfluoro-n-[1,2,3,4-13C4]octanoic acid (PFOA-13C4) | 4.70 | 416.9 | 372.0* | -30 | -15 | |
Perfluoro-n-[1,2,3,4,5-13C5]nonanoic acid (PFNA-13C5) | 5.39 | 467.9 | 422.9* | -19 | -14 | |
Perfluoro-n-[1,2-13C2]decanoic acid (PFDA-13C2) | 6.08 | 514.9 | 469.9* | -33 | -24 | |
Perfluoro-n-[1,2-13C2]undecanoic acid (PFUnDA-13C2) | 6.73 | 564.9 | 519.9* | -29 | -15 | |
Perfluoro-n-[1,2-13C2]dodecanoic acid (PFDoDA-13C2) | 7.32 | 614.8 | 569.9* | -20 | -19 | |
Sodium perfluoro-1-hexane[18O2]sulfonate (PFHxS-18O2) | 4.12 | 402.9 | 83.9* | -70 | -75 | |
Sodium perfluoro-1-[1,2,3,4-13C4]octanesulfonate (PFOS-13C4) | 5.42 | 502.9 | 79.9* | -60 | -96 |
图2 17种PFASs的MRM色谱图
Fig. 2 MRM chromatograms of the 17 PFASs 1. PFBA; 2. PFPeA; 3. PFBS; 4. PFHxA; 5. PFHpA; 6. PFHxS; 7. PFOA; 8. PFNA; 9. PFOS; 10. PFDA; 11. PFUnDA; 12. PFDS; 13. PFDoDA; 14. PFTrDA; 15. PFTeDA; 16. PFHxDA; 17. PFODA.
Compound | Linear equation | R2 | LOD/ (μg/kg) | LOQ/ (μg/kg) |
---|---|---|---|---|
PFBA | y=1.00849x+0.0727 | 0.9994 | 0.007 | 0.02 |
PFPeA | y=0.99373x+0.1413 | 0.9985 | 0.007 | 0.02 |
PFBS | y=1.69526x-0.0103 | 0.9992 | 0.007 | 0.02 |
PFHxA | y=0.84395x+0.1736 | 0.9917 | 0.003 | 0.01 |
PFHpA | y=1.02703x+0.2281 | 0.9915 | 0.007 | 0.02 |
PFHxS | y=1.16612x-0.0007 | 0.9980 | 0.007 | 0.02 |
PFOA | y=1.06944x+0.2209 | 0.9995 | 0.003 | 0.01 |
PFNA | y=0.94917x+0.1736 | 0.9941 | 0.003 | 0.01 |
PFOS | y=1.23867x+0.0096 | 0.9999 | 0.007 | 0.02 |
PFDA | y=0.49088x+0.0597 | 0.9997 | 0.003 | 0.01 |
PFUnDA | y=0.95842x-0.0013 | 0.9981 | 0.003 | 0.01 |
PFDS | y=0.58787x-0.0118 | 0.9958 | 0.007 | 0.02 |
PFDoDA | y=0.72798x-0.0007 | 0.9998 | 0.003 | 0.01 |
PFTrDA | y=0.69375x-0.0025 | 0.9981 | 0.003 | 0.01 |
PFTeDA | y=0.70892x-0.0190 | 0.9959 | 0.003 | 0.01 |
PFHxDA | y=0.37967x-0.0156 | 0.9970 | 0.007 | 0.02 |
PFODA | y=0.44318x-0.0719 | 0.9994 | 0.007 | 0.02 |
表2 17种PFASs的线性方程、相关系数、检出限和定量限
Table 2 Linear equations, correlation coefficients (R2), LODs and LOQs of the 17 PFASs
Compound | Linear equation | R2 | LOD/ (μg/kg) | LOQ/ (μg/kg) |
---|---|---|---|---|
PFBA | y=1.00849x+0.0727 | 0.9994 | 0.007 | 0.02 |
PFPeA | y=0.99373x+0.1413 | 0.9985 | 0.007 | 0.02 |
PFBS | y=1.69526x-0.0103 | 0.9992 | 0.007 | 0.02 |
PFHxA | y=0.84395x+0.1736 | 0.9917 | 0.003 | 0.01 |
PFHpA | y=1.02703x+0.2281 | 0.9915 | 0.007 | 0.02 |
PFHxS | y=1.16612x-0.0007 | 0.9980 | 0.007 | 0.02 |
PFOA | y=1.06944x+0.2209 | 0.9995 | 0.003 | 0.01 |
PFNA | y=0.94917x+0.1736 | 0.9941 | 0.003 | 0.01 |
PFOS | y=1.23867x+0.0096 | 0.9999 | 0.007 | 0.02 |
PFDA | y=0.49088x+0.0597 | 0.9997 | 0.003 | 0.01 |
PFUnDA | y=0.95842x-0.0013 | 0.9981 | 0.003 | 0.01 |
PFDS | y=0.58787x-0.0118 | 0.9958 | 0.007 | 0.02 |
PFDoDA | y=0.72798x-0.0007 | 0.9998 | 0.003 | 0.01 |
PFTrDA | y=0.69375x-0.0025 | 0.9981 | 0.003 | 0.01 |
PFTeDA | y=0.70892x-0.0190 | 0.9959 | 0.003 | 0.01 |
PFHxDA | y=0.37967x-0.0156 | 0.9970 | 0.007 | 0.02 |
PFODA | y=0.44318x-0.0719 | 0.9994 | 0.007 | 0.02 |
Compound | 0.05 μg/kg | 0.5 μg/kg | 1.8 μg/kg | ||||||
---|---|---|---|---|---|---|---|---|---|
Recovery/ % | RSD/ % | Recovery/ % | RSD/ % | Recovery/ % | RSD/ % | ||||
PFBA | 89.3 | 10.0 | 100.1 | 3.9 | 97.9 | 7.0 | |||
PFPeA | 88.9 | 9.1 | 81.4 | 2.5 | 83.9 | 9.7 | |||
PFBS | 104.0 | 4.6 | 103.7 | 9.3 | 105.2 | 6.8 | |||
PFHxA | 74.6 | 4.5 | 90.7 | 3.4 | 101.2 | 6.7 | |||
PFHpA | 127.1 | 5.7 | 123.6 | 4.8 | 116.9 | 0.8 | |||
PFHxS | 82.1 | 7.1 | 96.6 | 2.7 | 98.9 | 2.9 | |||
PFOA | 71.1 | 5.0 | 92.9 | 2.4 | 79.7 | 5.3 | |||
PFNA | 111.6 | 2.5 | 104.8 | 4.2 | 96.5 | 5.0 | |||
PFOS | 106.1 | 0.6 | 102.4 | 4.1 | 110.4 | 7.2 | |||
PFDA | 97.2 | 2.9 | 103.8 | 7.5 | 105.9 | 9.4 | |||
PFUnDA | 99.9 | 3.5 | 92.3 | 3.7 | 79.5 | 12.9 | |||
PFDS | 111.9 | 5.4 | 101.2 | 2.1 | 104.8 | 4.7 | |||
PFDoDA | 124.9 | 1.0 | 112.5 | 1.4 | 120.1 | 9.5 | |||
PFTrDA | 101.4 | 12.9 | 100.6 | 4.6 | 97.5 | 8.5 | |||
PFTeDA | 122.7 | 14.4 | 104.1 | 1.7 | 80.8 | 5.1 | |||
PFHxDA | 127.2 | 2.7 | 106.1 | 6.4 | 74.3 | 7.3 | |||
PFODA | 127.4 | 6.7 | 97.0 | 1.3 | 74.0 | 5.6 |
表3 17种PFASs的加标回收率和精密度(n=6)
Table 3 Spiked recoveries and RSDs of the 17 PFASs (n=6)
Compound | 0.05 μg/kg | 0.5 μg/kg | 1.8 μg/kg | ||||||
---|---|---|---|---|---|---|---|---|---|
Recovery/ % | RSD/ % | Recovery/ % | RSD/ % | Recovery/ % | RSD/ % | ||||
PFBA | 89.3 | 10.0 | 100.1 | 3.9 | 97.9 | 7.0 | |||
PFPeA | 88.9 | 9.1 | 81.4 | 2.5 | 83.9 | 9.7 | |||
PFBS | 104.0 | 4.6 | 103.7 | 9.3 | 105.2 | 6.8 | |||
PFHxA | 74.6 | 4.5 | 90.7 | 3.4 | 101.2 | 6.7 | |||
PFHpA | 127.1 | 5.7 | 123.6 | 4.8 | 116.9 | 0.8 | |||
PFHxS | 82.1 | 7.1 | 96.6 | 2.7 | 98.9 | 2.9 | |||
PFOA | 71.1 | 5.0 | 92.9 | 2.4 | 79.7 | 5.3 | |||
PFNA | 111.6 | 2.5 | 104.8 | 4.2 | 96.5 | 5.0 | |||
PFOS | 106.1 | 0.6 | 102.4 | 4.1 | 110.4 | 7.2 | |||
PFDA | 97.2 | 2.9 | 103.8 | 7.5 | 105.9 | 9.4 | |||
PFUnDA | 99.9 | 3.5 | 92.3 | 3.7 | 79.5 | 12.9 | |||
PFDS | 111.9 | 5.4 | 101.2 | 2.1 | 104.8 | 4.7 | |||
PFDoDA | 124.9 | 1.0 | 112.5 | 1.4 | 120.1 | 9.5 | |||
PFTrDA | 101.4 | 12.9 | 100.6 | 4.6 | 97.5 | 8.5 | |||
PFTeDA | 122.7 | 14.4 | 104.1 | 1.7 | 80.8 | 5.1 | |||
PFHxDA | 127.2 | 2.7 | 106.1 | 6.4 | 74.3 | 7.3 | |||
PFODA | 127.4 | 6.7 | 97.0 | 1.3 | 74.0 | 5.6 |
Samples | Buffer salt type | Purification method | LOD/(μg/kg) | Compound Mr | Ref. | |
---|---|---|---|---|---|---|
Fish | CH3COONH4 | WAX SPE | 0.06- | 0.19 | 214-614 | [ |
Aquatic products | CH3COONH4 | QuEChERS (C18+GCB) | 0.006- | 0.02 | 214-914 | [ |
Pork, beef, lamb | CH3COONH4 | QuEChERS (C18+PSA+GCB) | 0.02- | 0.05 | 214-700 | [ |
Crab meat | CH3COONH4 | m-PFC filtered SPE | 0.03- | 0.15 | 214-714 | [ |
Fish | CH3COONH4 | m-PFC filtered SPE | 0.015- | 0.05 | 214-714 | [ |
Beef | NH4F | d-SPE (C18+PSA+GCB+EMR-Lipid) | 0.003- | 0.007 | 214-914 | this study |
表4 本研究建立的检测方法与文献方法的比较
Table 4 Comparison between the detection method established in this study and published methods
Samples | Buffer salt type | Purification method | LOD/(μg/kg) | Compound Mr | Ref. | |
---|---|---|---|---|---|---|
Fish | CH3COONH4 | WAX SPE | 0.06- | 0.19 | 214-614 | [ |
Aquatic products | CH3COONH4 | QuEChERS (C18+GCB) | 0.006- | 0.02 | 214-914 | [ |
Pork, beef, lamb | CH3COONH4 | QuEChERS (C18+PSA+GCB) | 0.02- | 0.05 | 214-700 | [ |
Crab meat | CH3COONH4 | m-PFC filtered SPE | 0.03- | 0.15 | 214-714 | [ |
Fish | CH3COONH4 | m-PFC filtered SPE | 0.015- | 0.05 | 214-714 | [ |
Beef | NH4F | d-SPE (C18+PSA+GCB+EMR-Lipid) | 0.003- | 0.007 | 214-914 | this study |
图8 1份牛肉样品的MRM色谱图
Fig. 8 MRM chromatograms of a beef sample 1. PFBA-13C4; 2. PFHxA-13C2; 3. PFHxS-18O2; 4. PFOA-13C4; 5. PFNA-13C5; 6. PFOS-13C4; 7. PFDA-13C2; 8. PFUnDA-13C2; 9. PFDoDA-13C2; 10: PFOA.
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