鸡配合饲料中钙、磷元素标准物质研制

严华; 徐思远; 胡深; 张祯昊; 贾铮; 樊霞

doi:10.12338/j.issn.2096-9015.2023.0324

鸡配合饲料中钙、磷元素标准物质研制

doi: 10.12338/j.issn.2096-9015.2023.0324

严华^1,,
徐思远¹,
胡深²,
张祯昊¹,
贾铮¹,
樊霞¹

1.
中国农业科学院农业质量标准与检测技术研究所，北京 100081
2.
湖北省兽药监察所，武汉 430070

基金项目: 新疆维吾尔自治区“两区”科技发展计划项目（2023LQ02002）。

详细信息

作者简介:
严华（1978-），中国农业科学院农业质量标准与检测技术研究所副研究员，研究方向：饲料质量安全，邮箱：56431978@qq.com

中图分类号: TB99
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- 文章访问数: 83
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- PDF下载量: 10
- 被引次数: 0
出版历程
- 收稿日期: 2023-11-30
- 录用日期: 2023-12-04
- 修回日期: 2023-12-11
- 网络出版日期: 2023-12-15
- 刊出日期: 2023-10-18

Development of Reference Material for Calcium and Phosphorus in Chicken Formula Feed

1.
Institute of Quality Standard and Testing Technology for Agro-Products, Chinese Academy of Agricultural Sciences, Beijing 100081, China
2.
Hubei Province Institute of Veterinary Drug, Wuhan 430070, China

摘要

摘要: 研制了鸡配合饲料中钙、磷元素标准物质，使用微波消解进行样品前处理，电感耦合等离子体发射光谱仪（ICP-OES）对标准物质的钙、磷元素含量进行了定值，对样品的均匀性和稳定性进行了分析，评定了标准物质的不确定度。研究结果表明，鸡配合饲料标准物质样品具有良好的均匀性和稳定性，标准物质的钙含量标准值为1.221%，磷含量标准值为0.687%，扩展不确定度分别为0.117%和0.091%（k=2）。该标准物质的研制满足了饲料质量安全监测的需求，并为配合饲料中钙和磷元素分析的校准、质量控制和方法验证提供了技术支持。
- 计量学 /
- 鸡配合饲料 /
- 钙 /
- 磷 /
- 标准物质 /
- 定值 /
- 不确定度
Abstract: To address the needs of food safety monitoring, a certified reference material (CRM) for calcium and phosphorus in chicken formula feed was developed. The CRM underwent sample pretreatment using microwave digestion, followed by quantification of calcium and phosphorus content using an inductively coupled plasma optical emission spectrometer (ICP-OES). The homogeneity and stability of the CRM were systematically analyzed, and uncertainties were evaluated. The results demonstrate that the CRM exhibits excellent homogeneity and stability, with certified values of 1.221% for calcium and 0.687% for phosphorus, and expanded uncertainties of 0.117% and 0.091% (k=2), respectively. The CRM can be stored for 16 months at −18 ℃. This development fulfills the requirements for feed quality and safety monitoring and provides essential technical support for calibration, quality control, and method validation in the analysis of calcium and phosphorus in formulated feed samples.
- metrology /
- chicken formula feed /
- calcium /
- phosphorous /
- reference material /
- characterization /
- uncertainty

HTML全文

图 1 合并数据直方图及正态分布模拟曲线

Figure 1. Combined data histogram and normal distribution simulation curve

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表 1 微波消解程序

Table 1. Microwave digestion procedure for sample preparation

步骤	1	2	3	4	5
温度（℃）	80	100	150	170	190
保温时间（min）	3	3	5	5	25

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表 2 鸡配合饲料Ca和P均匀性统计分析结果

Table 2. Statistical analysis of calcium and phosphorus homogeneity in chicken formula feed

元素	平均值（%）	SD	RSD(%)	S₁²	S₂²	F值
Ca	1.253	0.05882	4.69	0.0043851	0.0030154	1.45
P	0.689	0.02953	4.29	0.0012561	0.0006873	1.83

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表 3 鸡配合饲料Ca和P标准物质短期稳定性（60℃）

Table 3. Short-term stability analysis of calcium and phosphorus in chicken formula feed CRM at 60℃

时间/天	Ca（%）			P（%）
0	1.209			0.694
1	1.251			0.672
2	1.270			0.692
3	1.223			0.698
6	1.217			0.700
平均值	1.234			0.691
$ \left\|{\beta }_{1}\right\| $	0.00147	$ {\beta }_{0} $	1.239	$ \left\|{\beta }_{1}\right\| $	0.00241	$ {\beta }_{0} $	0.683
s($ {\beta }_{1} $)	0.00513	t_{(0.95, n-2)}	3.18	s($ {\beta }_{1} $)	0.00176	t_{(0.95, n-2)}	3.18
结论	$ \left\|{\beta }_{1}\right\| $< t_{(0.95, n-2)}$ \times $s($ {\beta }_{1} $)			结论	$ \left\|{\beta }_{1}\right\| $< t_{(0.95, n-2)}$ \times $s($ {\beta }_{1} $)

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表 4 鸡配合饲料Ca和P标准物质短期稳定性（40℃）

Table 4. Short-term stability analysis of calcium and phosphorus in chicken formula feed CRM at 40℃

时间/天	Ca（%）			P（%）
0	1.262			0.707
1	1.227			0.687
2	1.217			0.686
3	1.259			0.684
6	1.246			0.679
平均值	1.242			0.688
$ \left\|{\beta }_{1}\right\| $	0.00058	$ {\beta }_{0} $	1.240	$ \left\|{\beta }_{1}\right\| $	0.00311	$ {\beta }_{0} $	0.698
s($ {\beta }_{1} $)	0.00390	t_{(0.95, n-2)}	3.18	s($ {\beta }_{1} $)	0.00124	t_{(0.95, n-2)}	3.18
结论	$ \left\|{\beta }_{1}\right\| $< t_{(0.95, n-2)}$ \times $s($ {\beta }_{1} $)			结论	$ \left\|{\beta }_{1}\right\| $< t_{(0.95, n-2)}$ \times $s($ {\beta }_{1} $)

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表 5 鸡配合饲料Ca和P标准物质长期稳定性

Table 5. Long-term stability of calcium and phosphorus in chicken formula feed CRM

时间/月	Ca（%）			P（%）
0	1.315			0.696
1	1.204			0.691
2	1.115			0.636
3	1.273			0.688
6	1.235			0.698
平均值	1.250			0.682
$ \left\|{\beta }_{1}\right\| $	0.00696	$ {\beta }_{0} $	1.268	$ \left\|{\beta }_{1}\right\| $	0.00348	$ {\beta }_{0} $	0.691
s($ {\beta }_{1} $)	0.00686	t_{(0.95, n-2)}	3.18	s($ {\beta }_{1} $)	0.00680	t_{(0.95, n-2)}	3.18
结论	$ \left\|{\beta }_{1}\right\| $< t_{(0.95, n-2)}$ \times $s($ {\beta }_{1} $)			结论	$ \left\|{\beta }_{1}\right\| $< t_{(0.95, n-2)}$ \times $s($ {\beta }_{1} $)

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表 6 鸡配合饲料Ca和P基体标准物质的定值结果

Table 6. Certification results for calcium and phosphorus in chicken formula feed CRM (%)

元素	1	2	3	4	5	6	7	8	9	平均值	标准偏差
Ca	1.245	1.213	1.213	1.214	1.226	1.198	1.240	1.223	1.216	1.221	0.0361
P	0.690	0.691	0.687	0.698	0.681	0.690	0.686	0.682	0.679	0.687	0.0174

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表 7 合成B类相对不确定度u_B,rel

Table 7. Composition and analysis of B-class relative uncertainty

元素	u_{m, rel}	u_d,rel	u_c,rel	u_cal,rel	u_B,rel
Ca	0.096	0.00311	0.267	0.63	0.69
P	0.096	0.00311	0.267	0.49	0.57

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表 8 鸡配合饲料中钙和磷元素标准物质的不确定度

Table 8. Uncertainty analysis for calcium and phosphorus in chicken formula feed CRM

元素	Ca	P
u_char,rel(%)	0.80	0.64
u_bb,rel(%)	1.70	2.00
u_s,rel(%)	4.39	6.21
$ {u}_{\mathrm{C}\mathrm{R}\mathrm{M},\mathrm{r}\mathrm{e}\mathrm{l}}\left(\mathrm{\%}\right) $	4.77	6.56
$ {U}_{\mathrm{C}\mathrm{R}\mathrm{M},\mathrm{r}\mathrm{e}\mathrm{l}} $(%)	9.55	13.1

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