新疆农业科学 ›› 2022, Vol. 59 ›› Issue (3): 674-682.DOI: 10.6048/j.issn.1001-4330.2022.03.017
张瑞1,2(), 苟春林3, 王智2, 乔坤云2, 袁玉伟4, 聂晶4, 琚艳君2, 赵多勇2()
收稿日期:
2021-08-15
出版日期:
2022-03-20
发布日期:
2022-03-28
通信作者:
赵多勇
作者简介:
张瑞(1997-),女,吉林松原人,硕士研究生,研究方向为食品加工与安全,(E-mail) 1761262569@qq.com
基金资助:
ZHANG Rui1,2(), GOU Chunlin3, WANG Zhi2, QIAO Kunyun2, YUAN Yuwei4, NIE Jing4, JU Yanjun2, ZHAO Duoyong2()
Received:
2021-08-15
Online:
2022-03-20
Published:
2022-03-28
Correspondence author:
ZHAO Duoyong
Supported by:
摘要:
【目的】比较新疆精河枸杞与宁夏中宁枸杞矿物元素含量差异,分析基于多元素分析技术鉴别枸杞产地的可行性,研究精河枸杞和中宁枸杞矿物元素指纹特征差异。【方法】采用电感耦合等离子质谱(ICP-MS)测定来自新疆精河县与宁夏中宁县2个产地的102份枸杞样品中52种矿物元素的含量,结合方差分析和正交偏最小二乘法-判别分析(OPLS-DA)等多元统计分析方法进行产地鉴别。【结果】精河枸杞和中宁枸杞中有26种矿物元素存在显著性差异(P<0.05),其中精河枸杞Mg、Al、P、K、V、Cu、Zn、As、Se、Mo、Ag、Cd、Gd、Er、Pb和U等16种元素含量显著高于中宁枸杞,而中宁枸杞Na、Ca、Ni、Rb、Sr、Hf、Ir、Au、Tl和Th等10种元素含量显著高于精河枸杞。逐步判别分析筛选出U、Mo、K、Rb、Au、Ir、Hf、Cu、Tl、Zn、Ca、Th、Mg和Cd等14种元素为差异显著元素变量,基于上述14种差异元素建立的多元素产地判别模型,对精河枸杞和中宁枸杞产地判别的准确率分别为100%和98.08%。【结论】精河枸杞和中宁枸杞具有各自独特的矿物元素指纹特征,利用多种矿物元素可有效鉴别新疆精河枸杞和宁夏中宁枸杞。
中图分类号:
张瑞, 苟春林, 王智, 乔坤云, 袁玉伟, 聂晶, 琚艳君, 赵多勇. 基于多种矿物元素的精河枸杞与中宁枸杞产地鉴别[J]. 新疆农业科学, 2022, 59(3): 674-682.
ZHANG Rui, GOU Chunlin, WANG Zhi, QIAO Kunyun, YUAN Yuwei, NIE Jing, JU Yanjun, ZHAO Duoyong. Geographical Origin Discrimination of Jinghe Wolfberry and Zhongning Wolfberry Based on Multi Mineral Elements Analysis[J]. Xinjiang Agricultural Sciences, 2022, 59(3): 674-682.
仪器名称 Name of instrument | 型号 Model | 生产厂家 Manufacturers |
---|---|---|
电感耦合等离子体质谱 ICP-MS | 7700X | 美国Agilent科技公司 |
微波消解仪 Microwave Digester | Mars240/50 | 美国CEM公司 |
超纯水仪 Ultra-pure water meter | Cascada III.I20 | 美国Pall公司 |
酸纯化仪 Acid Purification Instrument | DST-1000 | 美国Savillex公司 |
破壁机 Wall breaker | HR3868 | 荷兰Philips电子公司 |
电子天平 Electronic balance | XSE204 | 瑞士Mettler公司 |
表1 主要仪器设备及生产厂家
Table 1 Main instruments and manufacturers
仪器名称 Name of instrument | 型号 Model | 生产厂家 Manufacturers |
---|---|---|
电感耦合等离子体质谱 ICP-MS | 7700X | 美国Agilent科技公司 |
微波消解仪 Microwave Digester | Mars240/50 | 美国CEM公司 |
超纯水仪 Ultra-pure water meter | Cascada III.I20 | 美国Pall公司 |
酸纯化仪 Acid Purification Instrument | DST-1000 | 美国Savillex公司 |
破壁机 Wall breaker | HR3868 | 荷兰Philips电子公司 |
电子天平 Electronic balance | XSE204 | 瑞士Mettler公司 |
步骤 Steps | 温度 Temperature (℃) | 爬升时间 Climbing time (min) | 保持时间 Maintain time (min) | 功率 Power (W) | |
---|---|---|---|---|---|
升温 Heat up | 1 | 120 | 8 | 2 | 1 600 |
2 | 160 | 5 | 5 | 1 600 | |
降温 Cooling | 3 | 180 | 5 | 15 | 1 600 |
4 | - | 20 | - | - |
表2 微波消解参数条件
Table 2 Microwave digestion parameters
步骤 Steps | 温度 Temperature (℃) | 爬升时间 Climbing time (min) | 保持时间 Maintain time (min) | 功率 Power (W) | |
---|---|---|---|---|---|
升温 Heat up | 1 | 120 | 8 | 2 | 1 600 |
2 | 160 | 5 | 5 | 1 600 | |
降温 Cooling | 3 | 180 | 5 | 15 | 1 600 |
4 | - | 20 | - | - |
名称 Name | 参数 Parameter | 名称 Name | 参数 Parameter |
---|---|---|---|
RF功率 RF power | 1 350 W | 雾化室温度 Temperature of atomizing chamber | 2℃ |
采样深度 Sampling depth | 7.5 mm | 冷却气流速 Cooling gas velocity | 15 L/min |
辅助气流速 Auxiliary gas velocity | 1.0 L/min | 载气速度 Gas carrier velocity | 1.14 L/min |
氧化物指标 Oxide indicators | CeO+/Ce+<1.5% | 双电荷指标 Double charge indicator | Ce2+/Ce+<3% |
表3 ICP-MS工作条件
Table 3 Working parameters of ICP-MS
名称 Name | 参数 Parameter | 名称 Name | 参数 Parameter |
---|---|---|---|
RF功率 RF power | 1 350 W | 雾化室温度 Temperature of atomizing chamber | 2℃ |
采样深度 Sampling depth | 7.5 mm | 冷却气流速 Cooling gas velocity | 15 L/min |
辅助气流速 Auxiliary gas velocity | 1.0 L/min | 载气速度 Gas carrier velocity | 1.14 L/min |
氧化物指标 Oxide indicators | CeO+/Ce+<1.5% | 双电荷指标 Double charge indicator | Ce2+/Ce+<3% |
序号 Num | 元素 Elements | 新疆精河县 Jinghe County, Xinjiang (n=50) | 宁夏中宁县 Zhongning County, Ningxia (n=52) |
---|---|---|---|
$\bar{X}±S$ | X$\bar{X}±S$ | ||
1 | B | 2.04±0.45 | 1.99±0.30 |
2 | Na** | 601.31±205.24 | 842.18±450.94 |
3 | Mg** | 216.32±24.89 | 189.50±37.30 |
4 | Al** | 3 338.44±1 074.98 | 2 713.58±817.92 |
5 | P** | 561.45±73.54 | 504.86±91.12 |
6 | K** | 4 188.94±358.23 | 3 358.26±438.15 |
7 | Ca** | 180.83±44.81 | 225.77±56.05 |
8 | V** | 8.70±3.20 | 6.94±2.41 |
9 | Cr | 67.51±84.59 | 51.94±25.51 |
10 | Mn | 1 870.07±240.73 | 1 750.91±431.99 |
11 | Fe | 13.01±4.04 | 12.36±4.89 |
12 | Co | 11.17±4.16 | 10.06±3.23 |
13 | Ni** | 178.87±63.69 | 213.76±71.26 |
14 | Cu** | 2 126.10±616.73 | 1 385.47±662.86 |
15 | Zn** | 4 261.70±2 402.81 | 2 985.83±883.39 |
16 | As** | 5.72±1.91 | 4.75±1.49 |
17 | Se* | 18.48±20.08 | 11.66±4.86 |
18 | Rb** | 222.22±112.29 | 493.28±353.98 |
序号 Num | 元素 Elements | 新疆精河县 Jinghe County, Xinjiang (n=50) | 宁夏中宁县 Zhongning County, Ningxia (n=52) |
$\bar{X}±S$ | $\bar{X}±S$ | ||
19 | Sr* | 1 221.06±474.20 | 1 719.74±1 019.57 |
20 | Mo** | 77.01±18.71 | 35.23±11.06 |
21 | Pd | 0.82±0.31 | 0.83±0.32 |
22 | Ag* | 16.66±8.15 | 14.90±7.59 |
23 | Cd** | 14.77±6.51 | 11.00±9.06 |
24 | Sb | 1.07±0.70 | 1.06±0.72 |
25 | Cs | 1.2±0.47 | 1.58±1.15 |
26 | Ba | 199.58±74.93 | 216.85±80.20 |
27 | La | 4.96±1.91 | 4.75±1.87 |
28 | Ce | 5.75±3.21 | 5.09±2.68 |
29 | Pr | 1±0.45 | 0.87±0.34 |
30 | Nd | 3.88±1.77 | 3.45±1.29 |
31 | Sm | 0.73±0.37 | 0.66±0.28 |
32 | Eu | 0.13±0.08 | 0.11±0.06 |
33 | Gd* | 0.65±0.31 | 0.52±0.22 |
34 | Dy | 0.48±0.20 | 0.44±0.19 |
35 | Ho | 0.07±0.04 | 0.06±0.04 |
36 | Er** | 0.19±0.11 | 0.13±0.09 |
37 | Tm | 0.03±0.02 | 0.03±0.02 |
38 | Yb | 0.25±0.10 | 0.22±0.08 |
39 | Hf** | 1.26±0.44 | 1.96±0.70 |
40 | Ir** | 0.11±0.07 | 0.20±0.10 |
41 | Pt | 0.08±0.05 | 0.08±0.05 |
42 | Au** | 1.36±0.25 | 1.75±0.35 |
43 | Tl** | 0.26±0.20 | 0.40±0.18 |
44 | Pb** | 36.80±18.38 | 29.16±15.01 |
45 | Th** | 3.01±7.88 | 5.91±12.13 |
46 | U** | 1.76±0.42 | 0.71±0.22 |
表4 枸杞的46种元素含量
Table 4 Contents of 46 elements of wolfberry
序号 Num | 元素 Elements | 新疆精河县 Jinghe County, Xinjiang (n=50) | 宁夏中宁县 Zhongning County, Ningxia (n=52) |
---|---|---|---|
$\bar{X}±S$ | X$\bar{X}±S$ | ||
1 | B | 2.04±0.45 | 1.99±0.30 |
2 | Na** | 601.31±205.24 | 842.18±450.94 |
3 | Mg** | 216.32±24.89 | 189.50±37.30 |
4 | Al** | 3 338.44±1 074.98 | 2 713.58±817.92 |
5 | P** | 561.45±73.54 | 504.86±91.12 |
6 | K** | 4 188.94±358.23 | 3 358.26±438.15 |
7 | Ca** | 180.83±44.81 | 225.77±56.05 |
8 | V** | 8.70±3.20 | 6.94±2.41 |
9 | Cr | 67.51±84.59 | 51.94±25.51 |
10 | Mn | 1 870.07±240.73 | 1 750.91±431.99 |
11 | Fe | 13.01±4.04 | 12.36±4.89 |
12 | Co | 11.17±4.16 | 10.06±3.23 |
13 | Ni** | 178.87±63.69 | 213.76±71.26 |
14 | Cu** | 2 126.10±616.73 | 1 385.47±662.86 |
15 | Zn** | 4 261.70±2 402.81 | 2 985.83±883.39 |
16 | As** | 5.72±1.91 | 4.75±1.49 |
17 | Se* | 18.48±20.08 | 11.66±4.86 |
18 | Rb** | 222.22±112.29 | 493.28±353.98 |
序号 Num | 元素 Elements | 新疆精河县 Jinghe County, Xinjiang (n=50) | 宁夏中宁县 Zhongning County, Ningxia (n=52) |
$\bar{X}±S$ | $\bar{X}±S$ | ||
19 | Sr* | 1 221.06±474.20 | 1 719.74±1 019.57 |
20 | Mo** | 77.01±18.71 | 35.23±11.06 |
21 | Pd | 0.82±0.31 | 0.83±0.32 |
22 | Ag* | 16.66±8.15 | 14.90±7.59 |
23 | Cd** | 14.77±6.51 | 11.00±9.06 |
24 | Sb | 1.07±0.70 | 1.06±0.72 |
25 | Cs | 1.2±0.47 | 1.58±1.15 |
26 | Ba | 199.58±74.93 | 216.85±80.20 |
27 | La | 4.96±1.91 | 4.75±1.87 |
28 | Ce | 5.75±3.21 | 5.09±2.68 |
29 | Pr | 1±0.45 | 0.87±0.34 |
30 | Nd | 3.88±1.77 | 3.45±1.29 |
31 | Sm | 0.73±0.37 | 0.66±0.28 |
32 | Eu | 0.13±0.08 | 0.11±0.06 |
33 | Gd* | 0.65±0.31 | 0.52±0.22 |
34 | Dy | 0.48±0.20 | 0.44±0.19 |
35 | Ho | 0.07±0.04 | 0.06±0.04 |
36 | Er** | 0.19±0.11 | 0.13±0.09 |
37 | Tm | 0.03±0.02 | 0.03±0.02 |
38 | Yb | 0.25±0.10 | 0.22±0.08 |
39 | Hf** | 1.26±0.44 | 1.96±0.70 |
40 | Ir** | 0.11±0.07 | 0.20±0.10 |
41 | Pt | 0.08±0.05 | 0.08±0.05 |
42 | Au** | 1.36±0.25 | 1.75±0.35 |
43 | Tl** | 0.26±0.20 | 0.40±0.18 |
44 | Pb** | 36.80±18.38 | 29.16±15.01 |
45 | Th** | 3.01±7.88 | 5.91±12.13 |
46 | U** | 1.76±0.42 | 0.71±0.22 |
地点 Location | 样本量 Sample size | 识别率 Recognition(%) | 新疆精河县 Jinghe County, Xinjiang | 宁夏中宁县 Zhongning County, Ningxia |
---|---|---|---|---|
新疆精河县 Jinghe County, Xinjiang | 50 | 100% | 50 | 0 |
宁夏中宁县 Zhongning County, Ningxia | 52 | 98.08% | 1 | 51 |
表5 识别两产地枸杞评估
Table 5 Identification of evaluation form of wolfberry. from two areas
地点 Location | 样本量 Sample size | 识别率 Recognition(%) | 新疆精河县 Jinghe County, Xinjiang | 宁夏中宁县 Zhongning County, Ningxia |
---|---|---|---|---|
新疆精河县 Jinghe County, Xinjiang | 50 | 100% | 50 | 0 |
宁夏中宁县 Zhongning County, Ningxia | 52 | 98.08% | 1 | 51 |
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