电感耦合等离子体质谱仪测定酒类产品中钙、铬、锰、铁、镍、铜、锌、砷、镉、汞、铅的含量
GB 5009.268-2016《食品安全国家标准 食品中多元素的测定》【1】,其中第一法电感耦合等离子体质谱法,该法适用于食品中硼、钠、镁、铝、钾、钙、钛、钒、铬、锰、铁、钴、镍、铜、锌、砷、硒、锶、钼、镉、锡、锑、钡、汞、铊、铅的测定。现使用该检测方法测定酒类产品及其他食品中的钙、铬、锰、铁、镍、铜、锌、砷、镉、铅、汞的含量。元素 | 线性回归方程 | 相关系数 |
43Ca | Y=2929.280*X+7.522 | R2=0.9997 |
52Cr | Y=22044.402*X-990.976 | R2=0.9994 |
55Mn | Y=11055.215*X+60555.694 | R2=0.9984 |
57Fe | Y=482268.523*X+9366.720 | R2=1.0000 |
60Ni | Y=10096.186*X+3480.348 | R2=0.9997 |
63Cu | Y=22936.300*X+74473.941 | R2=0.9996 |
66Zn | Y=4024.051*X+20021.130 | R2=0.9996 |
75As | Y=1917.629*X+515.943 | R2=1.0000 |
111Cd | Y=9290.344*X-12.547 | R2=0.9999 |
202Hg | Y=25034.678*X+632.509 | R2=0.9993 |
208Pb | Y=141460.247*X+57969.253 | R2=0.9994 |
次数 | 1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 | 9 | 10 | 11 |
43Ca | 382.67 | 322.67 | 336.67 | 275.34 | 278.67 | 298.00 | 258.67 | 279.34 | 282.00 | 279.34 | 288.67 |
52Cr | 6250.94 | 6292.28 | 6625.12 | 6096.18 | 6169.55 | 6146.87 | 6106.85 | 6707.17 | 6498.39 | 6402.34 | 6186.23 |
55Mn | 4567.67 | 4052.74 | 3699.93 | 3321.80 | 3062.40 | 2999.71 | 3034.38 | 3198.43 | 3185.76 | 3132.41 | 3028.39 |
57Fe | 5972.80 | 5970.13 | 6170.89 | 5859.41 | 5884.75 | 5769.36 | 5691.99 | 6255.60 | 5979.46 | 5748.03 | 5991.47 |
60Ni | 1635.47 | 1405.43 | 1355.42 | 1246.07 | 1152.06 | 1156.06 | 1095.39 | 1218.73 | 1174.73 | 1170.06 | 1151.39 |
63Cu | 15760.61 | 14886.60 | 14233.63 | 12998.91 | 12931.45 | 12549.73 | 12541.70 | 13327.19 | 13133.00 | 12787.96 | 12807.29 |
66Zn | 12701.92 | 12395.57 | 12803.96 | 11999.16 | 12085.90 | 12226.05 | 12157.98 | 12795.94 | 12599.75 | 12315.48 | 12179.33 |
75As | 349.34 | 306.67 | 344.67 | 368.67 | 346.01 | 364.01 | 342.67 | 365.34 | 352.01 | 338.01 | 358.67 |
111Cd | 146.00 | 128.67 | 135.33 | 97.33 | 106.67 | 92.67 | 105.33 | 121.33 | 130.00 | 110.00 | 88.67 |
202Hg | 453.3 | 386.7 | 364.0 | 364.7 | 430.0 | 301.3 | 667.4 | 469.3 | 426.0 | 392.7 | 380.0 |
208Pb | 37472.44 | 35512.42 | 36409.83 | 32660.83 | 32421.57 | 32347.21 | 31364.48 | 34627.41 | 32826.39 | 32330.30 | 32438.76 |
43Ca | 1 | 2 | 3 | 4 | 5 | 6 | 平均值 | 相对标准偏差 |
测定低限 | 0.1387 | 0.1325 | 0.1483 | 0.1355 | 0.1443 | 0.1245 | 0.1373 | 6.2% |
一合适点 | 0.4062 | 0.4062 | 0.4247 | 0.3844 | 0.4225 | 0.4022 | 0.4077 | 3.6% |
常见限量 | 0.8221 | 0.8190 | 0.8241 | 0.8352 | 0.7717 | 0.8059 | 0.8130 | 2.7% |
52Cr | 1 | 2 | 3 | 4 | 5 | 6 | 平均值 | 相对标准偏差 |
测定低限 | 0.4244 | 0.4178 | 0.4104 | 0.4088 | 0.4085 | 0.3977 | 0.4113 | 2.2% |
一合适点 | 1.0214 | 1.0311 | 1.0169 | 1.0122 | 1.0743 | 0.9979 | 1.0257 | 2.6% |
常见限量 | 1.9993 | 2.0314 | 1.9942 | 2.0258 | 1.9618 | 2.0007 | 2.0022 | 1.2% |
55Mn | 1 | 2 | 3 | 4 | 5 | 6 | 平均值 | 相对标准偏差 |
测定低限 | 3.8766 | 3.8584 | 3.8297 | 3.9631 | 4.2706 | 3.7917 | 3.9317 | 4.5% |
一合适点 | 7.5686 | 7.3562 | 7.1860 | 7.4045 | 7.5246 | 7.2248 | 7.3775 | 2.1% |
常见限量 | 14.7415 | 15.1441 | 14.8418 | 15.0010 | 14.5963 | 14.6075 | 14.8220 | 1.5% |
57Fe | 1 | 2 | 3 | 4 | 5 | 6 | 平均值 | 相对标准偏差 |
测定低限 | 0.0079 | 0.0074 | 0.0065 | 0.0067 | 0.0071 | 0.0066 | 0.0070 | 8.2% |
一合适点 | 0.0649 | 0.0636 | 0.0638 | 0.0623 | 0.0663 | 0.0627 | 0.0640 | 2.3% |
常见限量 | 0.1664 | 0.1681 | 0.1675 | 0.1678 | 0.1645 | 0.1855 | 0.1700 | 4.6% |
60Ni | 1 | 2 | 3 | 4 | 5 | 6 | 平均值 | 相对标准偏差 |
测定低限 | 0.0244 | 0.0220 | 0.0160 | 0.0218 | 0.0209 | 0.0159 | 0.0202 | 17.0% |
一合适点 | 0.8343 | 0.8619 | 0.9113 | 0.8247 | 0.8574 | 0.8246 | 0.8524 | 3.9% |
常见限量 | 1.9073 | 1.9599 | 1.9439 | 1.9795 | 1.9037 | 1.9251 | 1.9366 | 1.6% |
63Cu | 1 | 2 | 3 | 4 | 5 | 6 | 平均值 | 相对标准偏差 |
测定低限 | 0.1979 | 0.1705 | 0.1469 | 0.1553 | 0.1595 | 0.1409 | 0.1618 | 12.6% |
一合适点 | 7.2305 | 7.2957 | 7.2005 | 7.1175 | 7.6566 | 7.0204 | 7.2535 | 3.0% |
常见限量 | 18.8729 | 18.8995 | 18.8277 | 18.2710 | 18.4932 | 18.2602 | 18.6041 | 1.6% |
66Zn | 1 | 2 | 3 | 4 | 5 | 6 | 平均值 | 相对标准偏差 |
测定低限 | 5.6130 | 5.5363 | 5.3177 | 5.4067 | 6.0297 | 5.3841 | 5.5479 | 4.7% |
一合适点 | 13.3356 | 12.8915 | 13.1220 | 13.0431 | 12.8157 | 12.7277 | 12.9893 | 1.7% |
常见限量 | 17.1946 | 17.3349 | 17.2263 | 17.1642 | 16.9062 | 16.5778 | 17.0673 | 1.6% |
75As | 1 | 2 | 3 | 4 | 5 | 6 | 平均值 | 相对标准偏差 |
测定低限 | 0.2181 | 0.1920 | 0.1804 | 0.2020 | 0.1886 | 0.1934 | 0.1958 | 6.6% |
一合适点 | 0.8852 | 0.9042 | 0.8438 | 0.8767 | 0.9778 | 0.8928 | 0.8968 | 5.0% |
常见限量 | 1.9963 | 2.2534 | 2.1336 | 2.1714 | 2.0149 | 1.9874 | 2.0928 | 5.2% |
111Cd | 1 | 2 | 3 | 4 | 5 | 6 | 平均值 | 相对标准偏差 |
测定低限 | 0.2283 | 0.2186 | 0.2162 | 0.2146 | 0.2110 | 0.2115 | 0.2167 | 2.9% |
一合适点 | 0.9260 | 0.9285 | 0.9236 | 0.9306 | 0.9629 | 0.9103 | 0.9303 | 1.9% |
常见限量 | 1.8738 | 1.9574 | 1.9297 | 1.9521 | 1.9139 | 1.8860 | 1.9188 | 1.8% |
202Hg | 1 | 2 | 3 | 4 | 5 | 6 | 平均值 | 相对标准偏差 |
测定低限 | 0.0626 | 0.0604 | 0.0604 | 0.0482 | 0.0533 | 0.0466 | 0.0553 | 12.4% |
一合适点 | 0.2619 | 0.2291 | 0.2394 | 0.2286 | 0.2540 | 0.2525 | 0.2442 | 5.7% |
常见限量 | 0.2440 | 0.2586 | 0.2659 | 0.2750 | 0.2776 | 0.2698 | 0.2652 | 4.7% |
208Pb | 1 | 2 | 3 | 4 | 5 | 6 | 平均值 | 相对标准偏差 |
测定低限 | 0.3544 | 0.3083 | 0.2969 | 0.3015 | 0.3016 | 0.2913 | 0.3090 | 7.4% |
一合适点 | 1.9196 | 1.8120 | 1.8240 | 1.7879 | 1.8954 | 1.8187 | 1.8429 | 2.8% |
常见限量 | 3.1208 | 3.3262 | 3.3047 | 3.3015 | 3.2807 | 3.2439 | 3.2630 | 2.3% |
元素 | 1 | 2 | 3 | 4 | 5 | 6 | 平均值 | 相对标准偏差 |
43Ca | 4.99 | 4.88 | 4.72 | 4.88 | 4.81 | 4.76 | 4.8 | 2.0% |
52Cr | 0.000698 | 0.000684 | 0.000658 | 0.000663 | 0.000675 | 0.000672 | 0.00067 | 2.2% |
55Mn | 0.0829 | 0.0825 | 0.0786 | 0.0803 | 0.0813 | 0.0812 | 0.081 | 1.9% |
57Fe | 0.0499 | 0.0485 | 0.0460 | 0.0474 | 0.0471 | 0.0480 | 0.048 | 2.8% |
60Ni | 0.000650 | 0.000636 | 0.000605 | 0.000603 | 0.000597 | 0.000613 | 0.00062 | 3.4% |
63Cu | 0.00224 | 0.00216 | 0.00192 | 0.00210 | 0.00201 | 0.00204 | 0.0021 | 5.4% |
66Zn | 0.00618 | 0.00590 | 0.00546 | 0.00572 | 0.00584 | 0.00577 | 0.0058 | 4.1% |
75As | 0.00347 | 0.00348 | 0.00333 | 0.00348 | 0.00336 | 0.00343 | 0.0034 | 1.9% |
111Cd | N.D. | N.D. | N.D. | N.D. | N.D. | N.D. | - | - |
202Hg | 0.00830 | 0.00775 | 0.00702 | 0.00798 | 0.00716 | 0.00699 | 0.0075 | 7.4% |
208Pb | 0.00146 | 0.00146 | 0.00141 | 0.00148 | 0.00145 | 0.00145 | 0.0015 | 1.5% |
标准物质 | 元素 | 标准值mg/kg | 实测值mg/kg | 平均值mg/kg | 相对标准偏差RSD/% |
蒜粉GBW10022 | Ca | 810±80 | 804.86 | 812.2 | 1.3 |
807.17 | |||||
824.42 | |||||
Cr | 0.30±0.07 | 0.272 | 0.27 | 4.1 | |
0.255 | |||||
0.275 | |||||
Mn | 13.4±0.8 | 13.45 | 13.3 | 2.3 | |
12.90 | |||||
13.41 | |||||
Fe | 205±18 | 191.63 | 192.4 | 2.0 | |
189.04 | |||||
196.51 | |||||
Ni | 0.92±0.11 | 0.828 | 0.82 | 2.0 | |
0.807 | |||||
0.839 | |||||
Cu | 4.6±0.4 | 4.15 | 4.2 | 1.6 | |
4.23 | |||||
4.10 | |||||
Zn | 21.7±1.4 | 20.64 | 20.6 | 0.53 | |
20.71 | |||||
20.50 | |||||
As | 0.31±0.04 | 0.290 | 0.30 | 2.4 | |
0.296 | |||||
0.304 | |||||
Cd | 0.062±0.003 | 0.0644 | 0.064 | 1.0 | |
0.0652 | |||||
0.0639 | |||||
Hg | 0.0040±0.0015 | 0.00292 | 0.0028 | 4.0 | |
0.00285 | |||||
0.00270 | |||||
Pb | 0.72±0.09 | 0.787 | 0.79 | 0.32 | |
0.790 | |||||
0.785 |