血清钾、钠、钙、镁离子色谱法候选参考测量程序的建立及性能评估

doi:10.3969/j.issn.1673-8640.2017.02.017

摘要/Abstract

摘要：

目的建立一种基于离子色谱技术的血清电解质（钾、钠、钙、镁）候选参考测量程序并评价其性能。方法采用一种简单的湿法消化方法对血清样本进行前处理,然后采用离子色谱仪检测。以患者新鲜血清及国际临床化学和检验医学联合会参考实验室外部质量评价计划（RELA）样本作为检测样本,对候选参考测量程序的正确度和不精密度进行评估,同时与决定性方法[电感耦合等离子体质谱法（ICP-MS）]比较。结果 2 mL硝酸可将1.0 mL血清样本中的蛋白完全去除。32 mmol/L甲基磺酸淋洗液能将钾、钠、钙、镁实现基线分离。建立的候选参考测量程序的正确度和不精密度均在1.0%以内,与ICP-MS具有良好的可比性。结论成功建立了基于离子色谱技术的检测血清钾、钠、钙、镁的候选参考测量程序,相对于ICP-MS,具有操作简便、运行成本低、正确度高、稳定性好等优点,在临床检验的量值溯源中更具实用价值。

关键词: 钾, 钠, 钙, 镁, 离子色谱法, 参考测量程序, 性能评估

Abstract:

Objective To establish a reference measurement procedure for the determination of serum electrolytes（potassium,sodium,calcium and magnesium） based on ion chromatography,and to evaluate its analytical performance.Methods Samples were prepared by a simple digestion and determined by ion chromatography. Fresh sample from patients and the International Federation of Clinical Chemistry and Laboratory Medicine External Quality Assessment Scheme for Reference Laboratories in Laboratory Medicine（RELA） sample were used. The accuracy,imprecision and methodology comparison with inductively coupled plasma mass spectrometry（ICP-MS） were evaluated.Results A total of 1.0 mL of serum sample was digested with 2 mL nitric acid. The samples were redissolved and determined by ion chromatography under the optimal eluent concentration of 32 mmol/L methane-sulfonic acid. The accuracy and imprecision were <1.0%. The results were comparable with the reference values obtained by ICP-MS. Conclusions The established reference measurement procedure for the determination of serum potassium,sodium,calcium and magnesium has the advantages of simple,low-cost,high accuracy and good stability compared to ICP-MS. It may provide an effective way for traceability.

Key words: Potassium, Sodium, Calcium, Magnesium, Ion chromatography, Reference measurement procedure, Performance evaluation

中图分类号:

R446.1

邹继华, 张曼, 沈敏, 屠敏敏, 张传宝, 闫颖, 邹炳德. 血清钾、钠、钙、镁离子色谱法候选参考测量程序的建立及性能评估[J]. 检验医学, 2017, 32(2): 143-148.

ZOU Jihua, ZHANG Man, SHEN Min, TU Minmin, ZHANG Chuanbao, YAN Ying, ZOU Bingde. Establishment and performance evaluation of candidate reference measurement procedure for the determination of serum potassium,sodium,calcium and magnesium based on ion chromatography[J]. Laboratory Medicine, 2017, 32(2): 143-148.

图/表 9

参考文献 15

[1]	.DA SILVA J A F,RICELLI N L,CARVALHO A Z,et al. Improved separation of IA and IIA metal cations in matrices with high sodium concentration by capillary electrophoresis with contactless conductometric detection[J]. J Braz Chem Soc,2003,14(2):265-268.
[2]	.陈文祥. 临床检验量值溯源与参考系统[J]. 中华检验医学杂志,2006,29(1):17-19.
[3]	.PANTEGHINI M.Traceability as a unique tool to improve standardization in laboratory medicine[J]. Clin Biochem,2009,42(4-5):236-240.
[4]	.VELAPOLDI R A,PAULE R C,SCHAFFER R,et al.A reference method for the determination of sodium in serum. NBS special publication 260-60[M]. Washington:US Department of Commerce/National Bureau of Standards,1978:1-94.
[5]	.VELAPOLDI R A,PAULE R C,SCHAFFER R,et al.A reference method for the determination of potassium in serum. NBS special publication 260-63[M]. Washington:US Department of Commerce/National Bureau of Standards,1979:1-89.
[6]	.LONG S E,VETTER T W.Determination of sodium in blood serum by inductively coupled plasma mass spectrometry[J]. J Anal At Spectrom,2002,17(12):1589-1594.
[7]	.MURPHY K E,LONG S E,REARICK M S,et al.The accurate determination of potassium and calcium using isotope dilution inductively coupled "cold" plasma mass spectrometry[J]. J Anal At Spectrom,2002,17(5):469-477.
[8]	.THIENPONT L M,VAN NUWENBORG J E,STCKL D. Ion chromatography as potential reference methodology for the determination of total sodium and potassium in human serum[J]. J Chromatogr A,1995,706(1-2):443-450.
[9]	.KLPMANN W R,RUSCHKE D,BTTNER J,et al.A candidate reference method for the determination of magnesium in serum[J]. J Clin Chem Clin Biochem,1989,27(1): 33-39.
[10]	.BROWN S S,HEALY M J,KEARNS M.BCR information. Report of the inter-laboratory trial of the reference method for the determination of total calcium in serum. Part Ⅰ[J]. J Clin Chem Clin Biochem,1981,19(6): 395-412.
[11]	.SIMPSON L A,HEARN R,MERSON S,et al.A comparison of double-focusing sector field ICP-MS,ICP-OES and octopole collision cell ICP-MS for the high-accuracy determination of calcium in human serum[J]. Talanta,2005,65(4):900-906.
[12]	.DEWITTE K,STCKL D,VAN DE VELDE M,et al. Evaluation of intrinsic and routine quality of serum total magnesium measurement[J]. Clin Chim Acta,2000,292(1-2):55-68.
[13]	.THIENPONT L M,VAN NUWENBORG J E,STCKL D. Ion chromatography as potential reference methodology for the determination of total calcium and magnesium in human serum[J]. Anal Chem,1994,66(14):2404-2408.
[14]	.邹炳德,邹继华,沈敏,等. 基于离子色谱法建立血清电解质参考测量程序[J]. 检验医学,2015,30(12):1250-1256.
[15]	.THIENPONT L M,VAN NUWENBORG J E,STCKL D. Ion chromatography as reference method for serum cations[J]. J Chromatogr A,1997,789:557-568.

梯度	钠	钾	钙	镁
1	0.000	0.000	0.000	0.000
2	1.304	0.103	0.050	0.021
3	2.609	0.205	0.100	0.042
4	3.913	0.308	0.150	0.063
5	5.217	0.410	0.200	0.083
6	6.522	0.513	0.250	0.104

梯度	钠	钾	钙	镁
1	0.000	0.000	0.000	0.000
2	1.304	0.103	0.050	0.021
3	2.609	0.205	0.100	0.042
4	3.913	0.308	0.150	0.063
5	5.217	0.410	0.200	0.083
6	6.522	0.513	0.250	0.104

项目	线性范围（mmol/L）	回归方程	r值	检出限（μmol/L）	定量限（μmol/L）
钠	0~6.527	Y=6.268 2X+0.009 8	1.000 0	0.019	0.063
钾	0~0.518	Y=6.776 3X-0.008 0	1.000 0	0.036	0.120
镁	0~0.104	Y=12.070 5X-0.004 4	0.999 9	0.030	0.100
钙	0~0.250	Y=12.820 3X+0.004 1	1.000 0	0.036	0.121

项目	线性范围（mmol/L）	回归方程	r值	检出限（μmol/L）	定量限（μmol/L）
钠	0~6.527	Y=6.268 2X+0.009 8	1.000 0	0.019	0.063
钾	0~0.518	Y=6.776 3X-0.008 0	1.000 0	0.036	0.120
镁	0~0.104	Y=12.070 5X-0.004 4	0.999 9	0.030	0.100
钙	0~0.250	Y=12.820 3X+0.004 1	1.000 0	0.036	0.121

项目	样本	测定值（mmol/L）	CV（%）	靶值（mmol/L）	偏移（%）	IFCC等效限（%）
钠	2014年RELA-A	137.621	0.16	138.260	-0.46	± 1.25
	2014年RELA-B	150.463	0.10	151.200	-0.49
	2015年RELA-A	140.149	0.09	139.588	0.40
	2015年RELA-B	154.268	0.11	154.200	0.04
钾	2014年RELA-A	5.848	0.39	5.878	-0.51	± 2.00
	2014年RELA-B	2.943	0.37	2.938	0.16
	2015年RELA-A	5.880	0.03	5.860	0.33
	2015年RELA-B	3.148	0.88	3.133	0.50
镁	2014年RELA-A	2.014	0.39	2.032	-0.87	± 3.75
	2014年RELA-B	0.978	0.78	0.983	-0.47
	2015年RELA-A	1.927	0.32	1.928	-0.01
	2015年RELA-B	0.909	0.54	0.908	0.08
钙	2014年RELA-A	3.165	0.44	3.153	0.38	± 2.50
	2014年RELA-B	1.826	0.18	1.826	0.01
	2015年RELA-A	3.022	0.12	3.026	-0.13
	2015年RELA-B	2.000	0.48	2.001	-0.05