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GB 5009.222-2016英文版

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标准编号: GB 5009.222-2016 (GB5009.222-2016)
中文名称: 食品安全国家标准 食品中桔青霉素的测定
英文名称: Determination of citrinin in Monascus products
行业: 国家标准
中标分类: X09
字数估计: 11,137
发布日期: 2016-12-23
实施日期: 2017-06-23
旧标准 (被替代): GB/T 5009.222-2008; SN/T 2426-2010; SN/T 2916-2011
标准依据: National Health and Family Planning Commission Notice No.17 of 2016

GB 5009.222-2016: 食品安全国家标准 食品中桔青霉素的测定
GB 5009.222-2016 英文名称: Determination of citrinin in Monascus products
中华人民共和国国家标准
1 范围
本标准规定了食品中桔青霉素的测定方法。
本标准第一法适用于大米、玉米、辣椒、红曲类产品中桔青霉素的测定,第二法适用于大米、大麦、燕麦、小麦中桔青霉素的测定。
第一法 免疫亲和柱净化-高效液相色谱法
5 分析步骤
5.1 提取
5.1.1 大米、玉米、辣椒
称取经充分粉碎均质试样10.0g(精确至0.1g)于150mL具塞锥形瓶中,加入50mL甲醇-水
(70+30)提取液,以高速均质器高速均质提取2min,过滤提取液,移取1.0mL滤液,置于另一干净的
容器中,加入49mL10mmol/L磷酸溶液(pH7.5)稀释、混匀;以玻璃纤滤纸过滤待免疫亲和柱净化。
5.1.2 红曲及其制品
称取经充分粉碎均质试样1.0g(精确至0.1g)于50mL具塞锥形瓶中,加入20mL甲醇-水
(70+30)提取液,以高速均质器高速均质提取2min,过滤提取液,移取1.0mL滤液,置于另一干净的
容器中,加入39mLPBS缓冲溶液稀释、混匀;以玻璃纤滤纸过滤待免疫亲和柱净化。
5.2 净化
5.2.1 大米、玉米、辣椒
将免疫亲和柱连接于10mL玻璃针筒下,准确移取10.0mL(相当于0.04g试样)上述澄清滤液过
免疫亲和柱,以1滴/s~2滴/s的流速全部通过亲和柱;加入5mL10mmol/L磷酸(pH7.5)以1滴/s~
2滴/s的流速淋洗柱子,直至空气进入到亲和柱中,弃去全部流出液。准确加入1.0mL洗脱液Ⅰ进行
洗脱,洗脱流速为1滴/s~2滴/s。收集全部洗脱液于玻璃试管中,供检测用。
5.2.2 红曲及其制品
将免疫亲和柱连接于10mL玻璃针筒下,准确移取10.0mL上述澄清滤液过免疫亲和柱,以1滴/s~
2滴/s的流速全部通过亲和柱;加入10mL0.1%吐温20-PBS溶液,以1滴/s~2滴/s的流速淋洗柱
子,直至空气进入到亲和柱中,弃去全部流出液。准确加入1.0mL洗脱液Ⅱ(红曲及其制品)进行洗
脱,洗脱流速为1滴/s~2滴/s。收集全部洗脱液于玻璃试管中,供检测用。
5.3 空白试验除不加试样外,均按上述操作步骤进行。
5.4 测定
5.4.1 液相色谱参考条件
5.4.1.1 大米、玉米、辣椒
液相色谱分析条件列出如下:
a) 色谱柱:C18柱,柱长150mm,内径4.6mm,粒径5μm,或等效柱;
b) 柱温:30℃;
c) 流速:1.0mL/min;
d) 进样量:50μL;
e) 检测条件:激发波长350nm,发射波长500nm;
f) 流动相A液:乙腈,流动相B液:10mmol/L磷酸(pH2.5)。
流动相及梯度洗脱条件见表1。
5.4.1.2 红曲及其制品
液相色谱分析条件列出如下:
a) 色谱柱:C18柱,柱长150mm,内径4.6mm,粒径5μm,或等效柱;
b) 柱温:30℃;
c) 流速:0.7mL/min;
d) 进样量:50μL;
e) 检测条件:激发波长350nm,发射波长500nm;
f) 流动相A液:乙腈,流动相B液:0.1%磷酸。
流动相及梯度洗脱条件见表2。
5.4.2 标准曲线的制作
配制0.0ng/mL、1.0ng/mL、2.0ng/mL、5.0ng/mL、10.0ng/mL、20.0ng/mL6个浓度的基质标
准工作液。在仪器最佳工作条件下,用基质标准工作溶液分别进样,以相应的桔青霉素的色谱峰的峰面
积为纵坐标,以基质标准工作溶液中桔青霉素的浓度为横坐标,绘制标准曲线。
桔青霉素标准的色谱图参见图A.1和图A.2。
5.4.3 试样溶液的测定
将试样溶液注入高效液相色谱仪,测定相应的峰面积。由标准曲线得到试样溶液中桔青霉素的
浓度。
7 精密度在重复条件下获得的两次独立测定结果的绝对差值不得超过算术平均值的10%。
8 其他
本方法中大米、玉米、辣椒粉样品的检出限和定量限分别为8μg/kg和25μg/kg;红曲及其制品的
检出限和定量限分别为25μg/kg和80μg/kg。
第二法 C18固相萃取小柱净化-高效液相色谱法
9 原理用乙腈-异丙醇-水的混合溶液提取试样中桔青霉素,C18固相萃取小柱净化,用配荧光检测器的液
相色谱仪测定,外标法定量。
10 试剂和材料除非另有说明,本方法所用试剂均为分析纯,水为GB 6682规定的二级水。
10.1 试剂
10.1.1 异丙醇(C3H8O):色谱纯。
10.1.2 乙腈(CH3CN):色谱纯。
10.1.3 磷酸(H3PO4):优级纯。
10.1.4 甲醇(CH3OH)。
10.2 试剂配制
10.2.1 提取溶剂:乙腈-异丙醇-水(35+10+55),用磷酸调pH为1.5。
10.2.2 磷酸溶液(0.08mol/L):取5.6mL磷酸,以水定容至1L。
10.2.3 流动相:乙腈-异丙醇-磷酸溶液(35+10+55)。
10.3 标准品
桔青霉素(C13H14O5,CAS号:518-75-2),纯度≥99%。或经国家认证并授予标准物质证书的标准物质。
10.4 标准溶液配制
10.4.1 桔青霉素标准储备液:称取适量桔青霉素标准物质,用乙腈溶解并定容至1.0mg/mL,0℃~4℃ 保存。
10.4.2 桔青霉素标准工作液:根据需要用流动相将标准储备液稀释成25ng/mL、50ng/mL、100ng/mL、
500ng/mL、1000ng/mL的标准工作溶液。
10.5.1 C18固相萃取柱:填料500mg,柱体积3mL,或等效柱。
10.5.2 玻璃纤维滤纸:直径11cm,孔径1.5μm。
11 仪器和设备
11.1 高效液相色谱仪:配有荧光检测器。
11.2 振荡器。
11.3 离心机:≥6500r/min。
11.4 真空固相萃取装置。
11.5 氮吹仪。
11.6 分析天平:感量0.0001g和0.01g。
12.1 提取
取样品500g,用粉碎机粉碎并通过830μm圆孔筛,混匀,分成2份,装入洁净容器内,密封保存。
称取试样约5g(精确至0.01g)于50mL离心管中,加10mL提取溶剂(10.2.1),在振荡器上振荡提取
30min。以3500r/min离心4min,上清液转入另一离心管中。在残渣中再加入5mL提取溶剂
(10.2.1),重复上述操作,合并上清液。在提取液中加水至40mL,并用磷酸调pH为1.5,过玻璃纤维滤纸,待净化。
12.2 净化
将上述溶液过预淋洗好的C18固相萃取柱,用5mL水淋洗柱子。待淋洗液全部流出柱子后,减压
抽干3min。用10mL甲醇以1.0mL/min的速度洗脱,收集全部洗脱液,在40℃下,N2 吹干,再以
1.0mL流动相溶解,过0.22μm的有机相微孔滤膜,供液相色谱测定。
除不加试样外,均按上述操作步骤进行。
12.4 测定
12.4.1 液相色谱参考条件
a) 色谱柱:C18柱,柱长250mm,内径4.6mm,粒径5μm,或等效者;
b) 流动相:乙腈-异丙醇-磷酸溶液(35+10+55);
c) 流速:1.0mL/min;
d) 进样量:50μL;
e) 柱温:28℃;
f) 检测波长:激发波长331nm,发射波长500nm。
根据样液中被测桔青霉素含量情况,选定峰面积相近的标准工作溶液。标准工作液和样液中桔青
霉素响应值均应在仪器检测线性范围内。对标准工作液和样液等体积参插进样测定。在上述色谱条件
下,桔青霉素保留时间约为9.1min,标准物质色谱图见图A.3。
在重复条件下获得的两次独立测定结果的绝对差值不得超过算术平均值的10%。
15 其他
方法检出限为3μg/kg,定量限为10μg/kg。
附 录 A
桔青霉素标准的液相色谱图
桔青霉素标准的液相色谱图见图A.1~图A.3。

GB 5009.222-2016
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
National Food Safety Standard -
Determination of Citrinin in Foods
ISSUED ON: DECEMBER 23, 2016
IMPLEMENTED ON: JUNE 23, 2017
Issued by: National Health and Family Planning Commission of the
People’s Republic of China;
China Food and Drug Administration.
Table of Contents
Foreword ... 3 
1 Scope ... 4 
2 Principle ... 4 
3 Reagents and materials ... 4 
4 Instruments and apparatuses ... 6 
5 Analysis steps ... 6 
6 Description of the analysis result ... 9 
7 Precision ... 9 
8 Others ... 10 
9 Principle ... 10 
10 Reagents and materials ... 10 
11 Instruments and apparatuses ... 11 
12 Analysis steps ... 11 
13 Description of the analysis result ... 12 
14 Precision ... 13 
15 Others ... 13 
Appendix A Liquid chromatogram of citrinin standard solution ... 14 
National Food Safety Standard -
Determination of Citrinin in Foods
1 Scope
This Standard specifies methods for the determination of citrinin in foods.
Method 1 of this standard is applicable to the determination of citrinin in rice,
corn, pepper and red yeast products; method 2 is applicable to the
determination of citrinin in rice, barley, oats and wheat.
Method 1 -- Immunoaffinity column purification - high
performance liquid chromatography
2 Principle
For the citrinin in the sample, use methanol-water to extract; filter and dilute the
extract; use the immunoaffinity column to purify; use the liquid chromatography
and the fluorescence detector to determine the content of citrinin; use the
external standard method to quantify.
3 Reagents and materials
Unless otherwise specified, all the reagents in this method are analytical
reagents; the water is grade-II water that is specified by GB/T 6682.
3.1 Reagents
3.1.1 Methanol (CH3OH): chromatographic pure.
3.1.2 Acetonitrile (CH3CH): chromatographic pure.
3.1.3 Phosphoric acid (H3PO4): chromatographic pure.
3.1.4 Glacial acetic acid (C2H4O2): chromatographic pure.
3.1.5 Sodium hydroxide (NaOH).
3.1.6 Tween-20 (C58H114O26).
3.4.2 Standard intermediate solution: accurately transfer 1.0 mL of the citrinin
standard stock solution in a 10 mL volumetric flask; use methanol to fix-volume;
the concentration is 10 μg/mL; store at 4°C.
3.4.3 Matrix standard working solution: according to the need, take an
appropriate amount of standard intermediate solution; use blank sample extract
to prepare matrix standard working solutions of different concentrations.
Prepare when needed.
3.5 Materials
3.5.1 Citrinin immunoaffinity column: column volume of 3 mL, maximum column
capacity of 20 ng, or equivalent column.
3.5.2 Glass-fiber filter paper: diameter of 11 cm; aperture of 1.5 μm.
4 Instruments and apparatuses
4.1 High performance liquid chromatography, with fluorescence detector.
4.2 Analytical balance: sensitivity of 0.000 1 g and 0.01 g.
4.3 High-speed homogenizer: ≥12 000 r/min.
4.4 Mixer.
5 Analysis steps
5.1 Extraction
Weigh 10.0 g (accurate to 0.1 g) of the fully pulverized homogeneous sample
into a 150 mL stoppered conical flask; add 50 mL of methanol-water (70+30)
extract; use high-speed homogenizer to extract for 2 min at high speed; filter
the extract; transfer 1.0 mL of the filtrate to another clean container; add 49 mL
of 10 mmol/L phosphoric acid solution (pH 7.5) to dilute and mix; use a glass-
fiber filter paper to filter the to-be-purified immunoaffinity column.
5.1.2 Red yeast and its products
Weigh 1.0 g (accurate to 0.1 g) of the fully pulverized homogeneous sample
into a 50 mL stoppered conical flask; add 20 mL of methanol-water (70+30)
the extract; transfer 1.0 mL of the filtrate to another clean container; add 39 mL
Prepare matrix standard working solutions of 6 concentrations, namely 0.0
ng/mL, 1.0 ng/mL, 2.0 ng/mL, 5.0 ng/mL, 10.0 ng/mL, and 20.0 ng/mL. Under
the optimal working conditions of the instrument, use the matrix standard
working solution for injection respectively; take the chromatographic peak area
of the corresponding citrinin as the ordinate, and the concentration of citrinin in
the matrix standard working solution as the abscissa to draw the standard curve.
See Figure A.1 and Figure A.2 for chromatograms of the citrinin standard.
5.4.3 Determination of sample solution
determine the corresponding peak area. Obtain the concentration of citrinin in
the sample solution from the standard curve.
6 Description of the analysis result
Calculate the content of citrinin in the sample according to Formula (1):
Where:
X -- the content of citrinin in the sample, in micrograms per kilogram (μg/kg);
ρ -- the concentration of citrinin in the sample solution, in micrograms per liter
(μg/L);
V -- constant volume, in milliliters (mL);
m -- the sample amount that is represented by the sample solution, in grams
(g).
The calculation result needs to be deducted from the blank value. The
calculation result shall keep two significant figures.
7 Precision
The absolute difference of two independent test results under repeatability
cannot exceed 10% of the arithmetic mean value.
10.3 Standard
Citrinin (C13H14O5, CAS No.: 518-75-2), purity ≥ 99%. or the standard substance
10.4 Preparation of standard solution
10.4.1 Citrinin standard stock solution: weigh an appropriate amount of citrinin
standard substance; use acetonitrile to dissolve and fix-volume to 1.0 mg/mL;
store at 0°C ~ 4°C.
10.4.2 Citrinin standard working solution: use the mobile phase to dilute the
standard stock solution into standard working solution of 25 ng/mL, 50 ng/mL,
100 ng/mL, 500 ng/mL, 1000 ng/mL as needed.
10.5 Materials
10.5.1 C18 solid phase extraction column: packing of 500 mg, column volume
10.5.2 Glass-fiber filter paper: diameter of 11 cm; aperture of 1.5 μm.
11 Instruments and apparatuses
11.1 High performance liquid chromatography, with fluorescence detector.
11.2 Oscillator.
11.3 Centrifuge: ≥ 6 500 r/min.
11.4 Vacuum solid-phase extraction device.
11.5 Nitrogen-blowing instrument.
11.6 Analytical balance: sensitivity of 0.000 1 g and 0.01 g.
12 Analysis steps
Take 500 g of sample; use a pulverizer to pulverize; pass through an 830 μm
round sieve; mix well; divide into 2 portions; place in a clean container; seal and
store. Weigh approximately 5 g (accurate to 0.01 g) of the sample into a 50 mL
centrifuge tube; add 10 mL of extraction solvent (10.2.1); extract for 30 min on
the shaker. Centrifugate at 3 500 r/min for 4 min; transfer the supernatant to
another centrifuge tube. Add another 5 mL of extraction solvent (10.2.1) to the
residue; repeat the above operation; combine the supernatant. Add water to the
   
相关标准:  GB 5009.225-2023  GB 5009.210-2023
 
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