Simultaneous Determination of 18 Elements in Caoxian Asparagus by Inductively Coupled Plasma-Mass Spectrometry

doi:10.11924/j.issn.1000-6850.casb2022-0666

Abstract

Abstract:

Asparagus is rich in nutrients, and Caoxian asparagus is popular because of its long history of planting and good quality. By establishing a method for determining the contents of 18 nutrient elements in asparagus by inductively coupled plasma-mass spectrometry (ICP-MS), the background value of nutrient elements in Caoxian asparagus was comprehensively analyzed. After the samples were microwave-digested by HNO₃-H₂O₂ peroxide, appropriate internal standard isotope elements were selected to improve the matrix effect and interference, and the 18 elements in Caoxian asparagus were determined by ICP-MS. The results showed that the linear range of Na, Mg and K in the mass concentration range of 0-20000 μg/L and Al, Ca, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, As, Se, Cd, Ba and Pb in the mass concentration range of 0-500 μg/L were good (r>0.9996), the precision of the instrument was concentrated in 0.34%-3.41%, and the recovery rate of standard addition was 88.35%-105.36%. The contents of Na, Mg, K and Ca in asparagus were at a relatively high level, and the content of Se was more abundant. This method is suitable for quick, sensitive and accurate determination of 18 elements in asparagus, and can provide data support for monitoring the background content of nutrient elements in Caoxian asparagus.

Key words: Caoxian County, asparagus, inductively coupled plasma-mass spectrometry, microwave digestion, elements

WANG Xiao, LI Xiaoming, SHAO Li, CHANG Chenyang. Simultaneous Determination of 18 Elements in Caoxian Asparagus by Inductively Coupled Plasma-Mass Spectrometry[J]. Chinese Agricultural Science Bulletin, 2023, 39(21): 126-132.

Figures/Tables 4

References 27

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工作参数	设定值
载气流量/(L/min)	0.8
补偿气流量/(L/min)	0.8
雾化室温度/℃	2
泵速/rps	0.1
提升速度/rps	0.3
提升时间/s	45
稳定时间/s	30
射频功率/W	1350
距管水平位/mm	0.5
距管垂直位/mm	0.0
采样锥材料	镍
灵敏度	Li≥3000；Y≥10000；l≥6000
氧化物(156/140)	≤2
双电荷(70/140)	≤3

工作参数	设定值
载气流量/(L/min)	0.8
补偿气流量/(L/min)	0.8
雾化室温度/℃	2
泵速/rps	0.1
提升速度/rps	0.3
提升时间/s	45
稳定时间/s	30
射频功率/W	1350
距管水平位/mm	0.5
距管垂直位/mm	0.0
采样锥材料	镍
灵敏度	Li≥3000；Y≥10000；l≥6000
氧化物(156/140)	≤2
双电荷(70/140)	≤3

元素	回归方程	相关系数	线性范围/(μg/L)	检出限/(mg/kg)	定量限/(mg/kg)	RSD/%
Na	Y=1796.7379X+52455.7033	1.0000	0 ~20000	1	3	1.93
Mg	Y=818.7239X+2259.9867	0.9999	0 ~20000	1	3	0.34
Al	Y=246.9980X+1833.8367	0.9999	0 ~500	0.5	2	1.45
K	Y=679.7096X+1343.7767	0.9999	0 ~20000	1	3	2.62
Ca	Y=23.9771X+74.0867	0.9996	0 ~500	1	3	2.15
V	Y=12989.7499X+95.5567	1.0000	0 ~500	0.002	0.005	1.31
Cr	Y=17740.6564X+776.7367	1.0000	0 ~500	0.05	0.2	1.36
Mn	Y=7625.4335X+1038.9933	1.0000	0 ~500	0.1	0.3	1.94
Fe	Y=14135.0826X+137626.8567	1.0000	0 ~500	1	3	1.52
Co	Y=33148.9216X+147.7833	1.0000	0 ~500	0.01	0.03	2.55
Ni	Y=9421.4031X+953.4367	1.0000	0 ~500	0.2	0.5	1.86
Cu	Y=25502.1804X+1924.7033	1.0000	0 ~500	0.05	0.2	1.30
Zn	Y=3490.2402X+2406.5733	0.9998	0 ~500	0.5	2	1.42
As	Y=2127.2927X+1263.2600	1.0000	0 ~500	0.01	0.03	1.41
Se	Y=110.5888X+1.9933	1.0000	0 ~500	0.01	0.03	2.36
Cd	Y=5874.1481X+42.7667	1.0000	0 ~500	0.002	0.005	1.70
Ba	Y=5570.2923X+2426.0600	1.0000	0 ~500	0.03	0.09	3.41
Pb	Y=85570.2589X+14442.1300	1.0000	0 ~500	0.02	0.05	2.18

元素	回归方程	相关系数	线性范围/(μg/L)	检出限/(mg/kg)	定量限/(mg/kg)	RSD/%
Na	Y=1796.7379X+52455.7033	1.0000	0 ~20000	1	3	1.93
Mg	Y=818.7239X+2259.9867	0.9999	0 ~20000	1	3	0.34
Al	Y=246.9980X+1833.8367	0.9999	0 ~500	0.5	2	1.45
K	Y=679.7096X+1343.7767	0.9999	0 ~20000	1	3	2.62
Ca	Y=23.9771X+74.0867	0.9996	0 ~500	1	3	2.15
V	Y=12989.7499X+95.5567	1.0000	0 ~500	0.002	0.005	1.31
Cr	Y=17740.6564X+776.7367	1.0000	0 ~500	0.05	0.2	1.36
Mn	Y=7625.4335X+1038.9933	1.0000	0 ~500	0.1	0.3	1.94
Fe	Y=14135.0826X+137626.8567	1.0000	0 ~500	1	3	1.52
Co	Y=33148.9216X+147.7833	1.0000	0 ~500	0.01	0.03	2.55
Ni	Y=9421.4031X+953.4367	1.0000	0 ~500	0.2	0.5	1.86
Cu	Y=25502.1804X+1924.7033	1.0000	0 ~500	0.05	0.2	1.30
Zn	Y=3490.2402X+2406.5733	0.9998	0 ~500	0.5	2	1.42
As	Y=2127.2927X+1263.2600	1.0000	0 ~500	0.01	0.03	1.41
Se	Y=110.5888X+1.9933	1.0000	0 ~500	0.01	0.03	2.36
Cd	Y=5874.1481X+42.7667	1.0000	0 ~500	0.002	0.005	1.70
Ba	Y=5570.2923X+2426.0600	1.0000	0 ~500	0.03	0.09	3.41
Pb	Y=85570.2589X+14442.1300	1.0000	0 ~500	0.02	0.05	2.18

元素	样品含量/(mg/kg)	加标水平/(mg/kg)	加标后含量/(mg/kg)	回收率/%	平均回收率/%	RSD/%
Na	4554.123	6	4559.050	82.11	88.35	4.50
	4550.000	12	4560.843	90.36
	4662.156	60	4717.698	92.57
Mg	125.135	6	131.328	103.21	94.75	6.22
	126.000	12	136.613	88.44
	124.872	60	180.438	92.61
Al	-	4	3.205	80.13	92.85	9.14
	-	8	7.778	97.22
	-	40	40.484	101.21
K	2295.580	6	2300.521	82.35	92.83	9.45
	2296.121	12	2307.027	90.88
	2300.110	60	2363.266	105.26
Ca	102.110	6	107.481	89.51	95.09	5.82
	98.210	12	109.327	92.64
	101.000	60	162.866	103.11
V	-	0.01	0.010	96.21	99.58	3.38
	-	0.02	0.021	104.21
	-	0.1	0.098	98.33
Cr	0.181	0.4	0.604	105.66	105.08	5.29
	0.179	0.8	1.069	111.25
	0.180	4	4.113	98.33
Mn	1.182	0.6	1.701	86.55	95.29	6.79
	1.179	0.12	1.294	96.22
	1.180	6	7.367	103.11
Fe	2.032	6	7.865	97.22	96.03	4.80
	2.111	12	14.259	101.23
	2.155	60	55.945	89.65
Co	-	0.06	0.050	82.56	91.07	6.57
	-	0.12	0.111	92.11
	-	0.6	0.591	98.55
Ni	-	1	1.031	103.11	96.97	5.71
	-	2	1.969	98.45
	-	10	8.936	89.36
Cu	1.285	0.4	1.714	107.21	105.36	5.24
	1.290	0.8	2.175	110.66
	1.286	4	5.215	98.22
Zn	1.381	4	5.111	93.25	101.08	6.29
	1.382	8	9.489	101.34
	1.380	40	44.840	108.65
As	-	0.06	0.050	82.66	91.44	8.17
	-	0.12	0.107	89.31
	-	0.6	0.614	102.34
Se	2.005	0.06	2.059	90.52	95.80	4.85
	2.110	0.12	2.171	102.23
	2.130	0.6	2.187	94.66
Cd	-	0.01	0.009	89.75	89.20	1.12
	-	0.02	0.018	90.21
	-	0.1	0.088	87.63
Ba	-	0.2	0.181	90.51	90.24	0.65
	-	0.4	0.357	89.35
	-	2	1.817	90.87
Pb	-	0.1	0.101	101.24	99.03	1.65
	-	0.2	0.195	97.28
	-	1	0.986	98.56