白酒中钒铬锰铁铜镍砷镉锑铅的测定编制说明.docx
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白酒中钒铬锰铁铜镍砷镉锑铅的测定编制说明
白酒中钒、铬、锰、铁、铜、镍、砷、镉、锑、铅的测定编制说明
白酒中钒、铬、锰、铁、铜、镍、砷、镉、锑、铅的测定
电感耦合等离子体质谱法（征求意见稿）
编制说明
一、标准起草的基本情况（包括简要的任务来源介绍、主要起草单位、起草人等）
本项目由贵州省卫生和计划生育委员会组织食品安全地方标准评审委员会专家组进行评审并通过立项，2015年5月11日以“卫计办函[2015]94号”下发任务。
由贵州茅台酒股份有限公司负责。
本标准主要起草单位为:
贵州茅台酒股份有限公司
本标准主要起草人为:
王莉、汪地强、赵振宇、曾稳稳、荣茂、龙薇运、江锋、聂叶、袁河、刘松、李清亮、胡容、饶书恺、申鹰。
二、编制过程（包括编制原则、各阶段工作过程等）
1、本标准的编制原则
1.1必要性:
白酒中无机元素的来源与酿造环境（土壤、粮食、水源）、酿造工艺、蒸馏工艺、蒸馏设备、陈酿工艺、勾兑、包装等环节密切相关，其含量的高低对产品品质具有重要影响。
该方法一次能快速测定各酿造环节易迁移的风险元素含量，对白酒行业具有重要意义。
1.2先进性:
该方法不需要传统的消解步骤，处理步骤简单并可实现一次性进样检测10种元素，大大提高检测效率，且将该技术应用到白酒检测并未有相关的国家标准。
2、工作过程
2.1立项批准
2014年6月3日，贵州省卫生和计划生育委员会下发《关于征集2014年贵州省食品安全地方标准制（修）订立项建议的函》（黔卫计函【2014】29号）。
我公司于2014年7月向卫计委提交立项申请，并于2014年8月向食品安全地方标准审评委员会相关专家进行项目申请说明。
2015年5月11日贵州省卫生和计划生育委员会办公室下发《省卫生计生委办公室关于同意<贵州苕粉>等25项贵州省食品安全地方标准立项的通知》（黔卫计办函【2015】94号）。
2.2任务落实
贵州茅台酒股份有限公司技术中心负责试验、起草标准文本;
贵州省分析测试研究院负责第一验证;
1
贵州省产品质量监督检测院负责第二验证;
贵州省质检院仁怀分院（国家酒检中心）负责第三验证。
起草工作计划于2016年5月前完成。
2.3、各阶段工作过程
1）2015年5月，在接到标准制定任务后，我们成立了《电感耦合等离子体质谱法检测白酒中无机元素》地方标准起草小组，明确起草人和工作任务。
2）2015年6月,2016年2月，根据前期大量的数据收集工作，以及对贵州省白酒酿造工艺的调查了解，分析各工艺环节易迁移进入白酒的10种风险无机元素，并从方法的线性、检出限、定量限、稳定性、准确度等方面进行条件试验，在此基础上编写了标准文本初稿。
3）2016年2月24日，在贵州省分析测试研究院召开标准起草讨论会，对标准文本初稿及样品的制备方面进行了探讨，确定方法验证实施方案。
4）2016年2月25日-3月7日，完成标准文本初稿修改完善和验证样品制备，在空白酒样的基础上约添加5ppb、50ppb、100ppb、500ppb的标液，Fe额外增加一个1000ppb的浓度梯度，各元素含量共设5个梯度，共计5份样品。
5）2016年3月8号~4月10号，三家方法验证单位（贵州省分析测试研究院、贵州省产品质量监督检测院、贵州省质检院仁怀分院（国家酒检中心））拿到统一制备的样品，分别按照标准文本初稿中的方法进行了验证，包括回收率、精密度、稳定性验证。
6）2016年4月，汇总分析验证数据，写标准编制说明，起草组根据验证情况召开讨论会，研究下一步工作。
7）2016年5月，组织公司技术委员会对标准文本进行审核，并对文本进行修改。
3、主要实验（或验证）的分析报告
现有的食品中无机元素的国标测定方法，其测定元素相对单一，工作量大，已经不满足现代企业对食品安全监控快速灵敏的要求，通过查阅大量国内外无机元素分析方法并进行比对分析，本方法采用ICP-MS对白酒中10种无机元素进行分析，这10种无机元素是前期大量的测量数据并结合行业实际情况而确定。
通过探讨样品中酒精等有机质对各无机元素响应值的干扰情况，最终省去了传统的消解步骤，直接将样品烘干除酒精，再用稀硝酸稀释，定容，上机进样分析，大大提高工作效率，并以回收率、精密度、稳定性对方法进行了验证，建立了白酒中钒、铬、锰、铁、铜、镍、砷、镉、锑、铅的测定方法。
将5个白酒试样分别称取11份，按上述分析方法测定10种无机元素含量，分析结果如下表1:
2
表1钒、铬、锰、铁、铜、镍、砷、镉、锑、铅含量分析结果单位:
mg/L元素VCrMnFeNiCuAsCdSbPb
0.01540.01040.03280.5340.01370.09400.01310.005850.005420.0101
0.01440.01070.03150.5070.01400.08970.01450.006000.005910.00970
0.01520.01050.03240.5100.01350.09360.01230.005850.005400.0101
0.01650.01050.03350.5230.01480.09340.01320.005810.004800.0103
0.01540.01060.03240.5150.01290.09660.01360.005210.005430.0106测
0.01540.01130.03250.5390.01160.09410.01390.005900.005610.0114定
样值0.01450.01050.03150.5440.01320.09240.01440.005860.005480.0105品0.01530.01040.03270.5030.01420.09090.01420.006000.006000.010110.01440.01030.03270.5330.01500.09250.01500.006010.005640.0113
0.01530.01050.03380.5420.01450.09360.01410.005860.005900.0106
0.01640.01140.03260.5200.01330.09770.01380.005300.005200.00980均0.01530.01060.03260.5250.01370.09350.01380.005790.005530.0104值
RS4.583.402.142.777.112.425.564.726.295.34D%
0.05880.05520.07870.6280.05910.1390.06140.05650.05030.0630
0.05580.05710.08110.6800.06040.1490.05800.05310.04830.0678
0.05910.05530.07950.6010.05690.1410.05990.05500.04500.0639
0.05890.05520.07620.6020.05900.1340.05060.05410.04860.0551
0.06270.05470.07850.6370.06330.1510.05910.05160.04910.0632测
0.05880.05620.07930.6790.05990.1390.05780.05500.05320.0638定
样值0.05600.05990.08350.6230.05890.1390.06020.05340.05040.0668
0.05900.05680.07930.6570.06610.1520.05830.05860.04960.0622品
0.06410.05800.08150.6600.06030.1400.05590.05480.04680.056920.05710.05640.07420.6750.05530.1320.06370.06220.04930.0637
0.05890.05110.07960.6430.05960.1380.06110.05680.05140.0693均0.05900.05600.07920.6440.05990.1410.05870.05560.04930.0632值
RS4.233.933.154.484.804.645.815.274.466.68D%
0.1080.1100.1230.5870.1130.1920.1230.1160.1090.100
0.1160.1150.1400.6660.1200.2040.1160.1230.1130.109
0.1120.1090.1220.5980.1080.2000.1300.1170.1010.110样测
0.1100.1090.1430.6310.1150.1980.1280.1220.1120.101品定0.1140.1150.1220.6180.1270.2040.1190.1190.1080.1073值0.1100.1090.1360.5650.1140.2000.1290.1150.1100.114
0.1090.1130.1260.5980.1060.2030.1230.1150.1010.103
0.1100.1130.1290.6410.1190.1930.1280.1250.1070.111
3
0.1150.1090.1380.6450.1180.1950.1310.1160.1150.107
0.1140.1170.1420.6760.1290.1980.1280.1180.1130.115
0.1150.1150.1390.5990.1190.2100.1170.1240.1100.109均0.1120.1120.1330.6200.1170.2000.1250.1190.1090.108值
RS2.462.866.295.565.962.734.313.264.264.49D%
0.5320.5300.5431.050.5330.6340.5600.5610.5360.453
0.5410.5400.5581.100.5410.5880.5970.5740.5650.429
0.5230.5530.5331.040.5130.6280.5840.5500.5430.458
0.5400.5330.5511.060.5340.6310.5900.5740.5010.457
0.5360.5340.5481.080.5380.6290.5480.5670.5330.450测
定0.5630.5390.5491.100.5400.6300.5770.5630.5150.460样值0.5310.5730.5451.050.5290.6630.6100.6130.5560.457
品0.5330.5380.5581.090.5490.6350.5600.5610.5330.427
0.5460.5100.5631.090.5400.6290.5870.5680.5380.45440.5400.5340.5581.150.5330.6540.5690.5770.5500.455
0.5380.5290.5451.030.5610.6430.5400.5930.5630.460均0.5380.5370.5501.080.5370.6330.5750.5730.5390.451值
RS1.922.901.563.122.232.953.743.023.582.59D%
0.01990.01670.03671.660.01870.09920.01930.01180.01120.0161
0.02000.01580.04051.570.01940.09200.02050.01210.01150.0161
0.02090.01650.03721.640.01990.09750.02150.01200.01200.0150
0.01950.01650.03681.660.01790.08970.01930.01080.01120.0161测0.01970.01680.04011.570.01850.09750.02010.01140.01140.0153定0.02010.01670.03771.650.01930.1030.01780.01220.01060.0162样值0.02070.01770.03491.660.02040.09930.01910.01230.01120.0176
品0.01980.01680.03661.580.01890.09840.02040.01170.01150.0161
0.02060.01620.03941.660.01910.09720.02210.01080.01130.015050.01980.01750.04171.690.01890.09050.01940.01250.01080.0173
0.02080.01690.03581.610.01860.10020.01890.01280.01190.0162均0.02020.01670.03791.630.01900.09670.01990.01190.01130.0161值
RS2.483.265.682.603.614.336.145.453.625.13D%
由以上结果可以看出，对5个不同浓度的白酒样品平行测定11次，相对标准偏差为1.56%,7.11%，符合分析要求。
本方法稳定，操作简便，适用范围广，满足白酒中钒、铬、锰、铁、铜、镍、砷、镉、锑、铅的含量分析。
4个实验室参与了本标准的比对验证，对5个不同浓度的样品进行了分析，结果见表2。
4
表2对比样品分析结果单位:
mg/L元素VCrMnFeNiCuAsCdSbPb
0.01450.009600.03010.4920.01260.08710.01410.005500.005400.00950
0.01480.009800.02960.5180.01380.08810.01290.005400.005600.00960
0.01410.01080.03320.4940.01250.09750.01280.005800.005100.00990
0.01460.01020.03010.4990.01310.08890.01280.005400.005200.0101贵州
0.01490.009900.02970.5210.01420.08760.01320.005600.005500.00970省分
析测0.01520.009600.03080.5010.01290.08890.01340.005700.005300.00960试研0.01540.01030.03100.4970.01360.08840.01290.005800.005700.00980究院0.01570.01030.02990.5210.01440.08960.01270.005800.005200.00990
0.01580.01060.03360.5170.01280.08750.01390.005500.005400.0101
0.01450.01020.03110.4960.01370.09020.01310.006100.005800.00960
0.01560.009700.02970.5100.01380.09910.01490.005600.005200.0107
0.01450.01020.03100.5090.01380.09270.01300.005500.005600.00990
0.01420.009800.03120.4990.01270.08920.01270.005600.005400.0104
0.01460.009600.02960.4940.01240.1010.01290.005500.005200.0101贵州0.01520.009800.03220.5470.01320.09140.01430.005900.005200.00980省产0.01460.01040.03150.5120.01370.08760.01350.006100.005700.0103品质0.01430.01010.03260.5310.01310.09240.01310.006000.005400.00950量监0.01470.009600.03390.5120.01360.09750.01330.005800.005200.00970督检样0.01450.009700.03080.4990.01410.09270.01280.005700.005100.0101验院品0.01430.01060.03240.5430.01400.08970.01310.005500.005600.010610.01440.01070.03370.5120.01340.09480.01290.005700.005100.00980
0.01570.01120.02990.5130.01320.09040.01440.006200.005300.00990
0.01570.009800.03010.4980.01380.1020.01420.005900.005900.0109
0.01490.01120.03520.5510.01420.09840.01290.006200.006100.0112贵州0.01560.01130.03450.5390.01460.08760.01450.006400.005800.0113省产0.01450.01100.03190.5490.01410.09960.01380.006300.005900.0107品质0.01630.01070.03470.5510.01280.09450.01470.006000.005700.00990量监0.01690.009900.03380.5450.01460.09870.01330.006100.006100.0112督检0.01610.01150.02980.5400.01470.1020.01270.006400.006200.0108验院0.01590.01140.03420.4970.01390.09810.01390.005800.005800.0112仁怀0.01650.01080.03290.5170.01260.09720.01420.006100.005900.0111分院0.01620.01010.03520.5380.01450.08880.01450.006300.005700.00980
0.01570.01120.03150.5560.01470.09630.01280.006200.006100.0108
0.01540.01040.03280.5340.01370.09400.01310.005850.005420.0101贵州
0.01440.01070.03150.5070.01400.08970.01450.006000.005910.00970茅台
酒股0.01520.01050.03240.5100.01350.09360.01230.005850.005400.0101份有0.01650.01050.03350.5230.01480.09340.01320.005810.004800.0103限公0.01540.01060.03240.5150.01290.09660.01360.005210.005430.0106
5
司0.01540.01130.03250.5390.01160.09410.01390.005900.005610.0114
0.01450.01050.03150.5440.01320.09240.01440.005860.005480.0105
0.01530.01040.03270.5030.01420.09090.01420.006000.006000.0101
0.01440.01030.03270.5330.01500.09250.01500.006010.005640.0113
0.01530.01050.03380.5420.01450.09360.01410.005860.005900.0106
0.01640.01140.03260.5200.01330.09770.01380.005300.005200.00980
0.05810.05510.07310.6170.05780.1380.05880.05860.04740.0621
0.05750.05460.07770.6320.05690.1310.05490.05450.04550.0604
0.05660.05180.07820.6080.06350.1340.05740.05390.04710.0582
0.0582
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