Scientia Agricultura Sinica ›› 2021, Vol. 54 ›› Issue (5): 1055-1062.doi: 10.3864/j.issn.0578-1752.2021.05.016

• FOOD SCIENCE AND ENGINEERING • Previous Articles     Next Articles

Determination of 5 Nitropolycyclic Aromatic Hydrocarbons in Roasted Meat Products by High Performance Liquid Chromatography- Fluorescence Detection

Xue BAI1,2(),Teng HUI2,ZhenYu WANG2,YunGang CAO1(),DeQuan ZHANG2()   

  1. 1School of Food and Biological Engineering, Shaanxi University of Science & Technology, Xi’an 710021;
    2Institute of Food Science and Technology, Chinese Academy of Agricultural Sciences/Key Laboratory of Agro-Products Processing, Ministry of Agriculture and Rural Affairs, Beijing 100193
  • Received:2020-06-29 Accepted:2020-09-15 Online:2021-03-01 Published:2021-03-09
  • Contact: YunGang CAO,DeQuan ZHANG E-mail:xuebai0527@163.com;caoyungang@sust.edu.cn;dequan_zhang0118@126.com

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Abstract:

【Objective】 This study was aimed to establish an approach to determine the content of five NPAHs (including 1-nitronaphthalene, 2-nitrofluorene, 3-nitrofluoranthene, 1-nitropyrene and 6-nitrobenzo[a]pyrene) in roasted meat based on solid-phase extraction (SPE) column and high performance liquid chromatography with fluorescence detection (HPLC-FLD).【Method】 1 g vacuum freeze-dried roasted meat sample was extracted by dichloromethane for ultrasonic extraction, and the filtrate was collected. Both the extraction and filtration processes were repeated three times. Then, the filtrate was dried by nitrogen and dissolved in 3 mL n-hexane. After that, the extract was loaded onto PAHs SPE column which was previously activated by dichloromethane and n-hexane. After loading, the sample tube was rinsed by n-hexane and loaded as well. The SPE column was washed by n-hexane and eluted by dichloromethane. The eluent was dried by nitrogen, and the residue was dissolved in acetonitrile to obtain NPAHs solution. Acidified methanol and iron powder were added to the NPAHs solution and heated in water bath with magnetic stirring for 40 min. After centrifugation and filtration, 20 μL sample was tested by HPLC-FLD at 40℃ by using Agilent ZORBAX Eclipse PAH analysis column. In the gradient elution system, water and acetonitrile were used as the mobile phases.【Result】 The result showed that five NPAHs were linear with correlation coefficients greater than 0.9940. Specifically, the detection limits (LOD) were within 0.12-2.17 μg·kg-1, and the quantification limits (LOQ) were within 0.38-7.23 μg·kg -1. The average recoveries and the precision were within 53.16%-129.64% and 1.91%-30.73%, respectively. Furthermore, five kinds of typical Chinese roasted meat products were tested by this method, and the content of five NPAHs in all roasted meat samples were between 50.19-82.36 μg·kg -1. Among them, the content of 6-nitrobenzo[a]pyrene was the highest, about 31.01-35.89 μg·kg-1, followed by 3-nitrofluoranthene, and the content was within the range of 9.99-23.06 μg·kg -1. 【Conclusion】 SPE column combined with HPLC-FLD was a suitable method to analyze NPAHs in roasted meat products; and NPAHs were widely contained in Chinese roasted meat products.

Key words: nitropolycyclic aromatic hydrocarbon, roasted meat products, high performance liquid chromatography-fluorescence detection, solid-phase extraction

Table 1

Gradient elution procedure of HPLC"

时间
Time (min)		 水
Water (%)		 乙腈
Acetonitrile (%)
0 70 30
20 0 100
25 0 100
30 70 30
35 70 30

Table 2

Detection procedure of fluorescence detector"

时间
Time (min)		 激发波长
Excitation wavelength (nm)		 发射波长
Emission wavelength (nm)		 硝基多环芳烃
NPAHs
0 240 430 1-NN
10 280 370 2-NF
13.4 300 530 3-NF
14 240 435 1-NP
16 432 502 6-NBAP

Fig. 1

HPLC chromatogram of NPAHs mixed standard solution (50 ng?mL-1) a：1-NN;b：2-NF;c：3-NF;d：1-NP;e：6-NBAP"

Table 3

Linear equation, correlation coefficient, LOD and LOQ of 5 NPAHs"

硝基多环芳烃 NPAHs 线性方程 Linear equation 相关系数 r 检出限 LOD 定量限 LOQ
1-硝基萘 1-NN y=1.5533x-0.1532 0.9941 0.20 0.69
2-硝基芴 2-NF y=1.7404x+0.0286 0.9989 0.22 0.74
3-硝基荧蒽 3-NF y=0.1666x+0.0218 0.9991 0.79 2.63
1-硝基芘 1-NP y=2.4321x-3.0797 0.9990 0.12 0.38
6-硝基苯并[a]芘 6-NBAP y=0.1101x-0.3392 0.9950 2.12 7.23

Table 4

Recovery and precision of method"

添加浓度
Added concentration
(ng?g-1)		 硝基多环芳烃NPAHs
1-硝基萘 1-NN 2-硝基芴 2-NF 3-硝基荧蒽 3-NF 1-硝基芘 1-NP 6-硝基苯并[a]芘 6-NBAP
回收率Recovery
(%)		 精密度
Precision
(%)		 回收率Recovery
(%)		 精密度Precision
(%)		 回收率Recovery
(%)		 精密度Precision
(%)		 回收率Recovery
(%)		 精密度Precision
(%)		 回收率Recovery
(%)		 精密度Precision
(%)
20 66.32 1.91 71.62 7.97 82.25 7.75 60.76 2.94 119.60 30.73
60 56.06 4.90 63.43 7.58 71.42 8.48 53.95 5.44 110.20 18.06
100 57.67 5.34 53.16 3.08 75.23 16.30 57.06 5.14 129.64 12.63

Table 5

Detection results of NPAHs in roasted meat products"

检测样品
Sample		 配料中有无NaNO2
NaNO2 in ingredients		 1-硝基萘
1-NN
(μg?kg-1)		 2-硝基芴
2-NF
(μg?kg-1)		 3-硝基荧蒽
3-NF
(μg?kg-1)		 1-硝基芘
1-NP
(μg?kg-1)		 6-硝基苯并[a]芘
6-NBAP (μg?kg-1)		 总硝基多环
芳烃
ΣNPAHs (μg?kg-1)
北京烤鸭1-胸肉
Beijing roasted duck 1-Breast meat		 有 Yes 2.93±0.77b 14.56±4.95a ND 12.89±0.16bc 31.72±1.29b 70.41±4.18ab
北京烤鸭1-胸皮
Beijing roasted duck 1-Breast skin		 有 Yes 3.19±1.21b 12.76±4.52ab 23.06±4.37a 13.80±1.27ab 31.14±0.24b 82.36±8.92a
北京烤鸭1-腿肉
Beijing roasted duck 1-Leg meat		 有 Yes 3.41±0.48b 11.71±6.16ab 16.92±1.85abc 12.85±0.08bc 35.89±0.31a 71.18±9.66ab
北京烤鸭1-腿皮
Beijing roasted duck 1-Leg skin		 有 Yes 3.64±0.22b 8.91±3.36ab 20.09±7.08abc 13.22±1.09abc 31.83±0.84b 71.92±4.51ab
北京烤鸭2-胸肉
Beijing roasted duck 2-Breast meat		 无 No 3.56±0.26b 14.71±0.87a ND 13.50±1.15abc 31.01±0.17b 77.72±1.65a
北京烤鸭2-胸皮
Beijing roasted duck 2-Breast skin		 无 No 3.90±1.02b 10.67±2.56ab ND 12.75±0.10c 31.02±0.22b 56.39±0.42bc
北京烤鸭2-腿肉
Beijing roasted duck 2-Leg meat		 无 No ND 9.32±3.76ab ND 12.89±0.14c 31.26±0.46b 58.01±2.78bc
北京烤鸭2-腿皮
Beijing roasted duck 2-Leg skin		 无 No 3.81±0.40b 8.33±2.81ab ND 13.38±0.81abc 31.20±0.32b 55.90±2.50bc
烤羊腿1 Roasted lamb leg 1 有 Yes 3.86±0.69b 9.15±2.86ab 21.16±7.82ab 13.95±0.92a 31.18±0.24b 70.32±7.57ab
烤羊腿2 Roasted lamb leg 2 无 No 10.39±6.07a 11.73±6.68ab 13.35±0.95bc 13.29±0.79abc 31.06±0.21b 64.00±5.81abc
烤猪肉片1 Roasted pork slice 1 有 Yes 3.22±0.26b 7.93±4.94ab 19.80±5.67ab 13.60±0.37abc 31.13±0.28b 68.55±4.88abc
烤猪肉片2 Roasted pork slice 2 无 No 5.77±0.65b 10.33±3.42ab 21.11±5.76ab 12.90±0.16bc 31.07±0.23b 67.73±3.27abc
烤鸡翅1 Roasted chicken wing 1 有 Yes 3.56±0.20b 10.54±3.12ab 9.99±0.99c 12.88±0.26bc 31.29±0.27b 58.63±2.58bc
烤鸡翅2 Roasted chicken wing 2 无 No 5.93±0.20b 8.80±1.31ab ND 13.06±0.72abc 31.75±0.68b 66.84±2.42abc
烤羊肉串1 Shish kebab 1 无 No 3.91±0.69b 7.25±1.54b ND 12.95±0.33bc 31.45±1.28b 55.56±1.13bc
烤羊肉串2 Shish kebab 2 无 No ND 5.84±0.57b ND 13.22±0.31abc 31.07±0.25b 50.19±0.53c
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