【讨论】稻瘟灵残留分析方法翻译求证

烘和灼烧是不一样的，我觉得第一个burn是对的，第二个burn应该改成dry。

标准溶液直接用standard solution就行了，为什么要加一个sample？

用丙酮配制成1.0mg／mL的标准储备液－－dilute with acetone to prepare a standard stock solution of 1.0 mg/ml.

临用时用丙酮稀释成1.0μg／mL的标准使用液。

我以前翻译都是两个都用burn,看来是错误的。

习惯了，还是应该翻译为test solution, standard solution，
我把那个浓度给看丢了。
多谢。

提取
称取20.0g经粉碎并过20目筛的大米样品置具塞锥形瓶中，加入50mL丙酮，于电动振荡器上振荡30min，用快速定性滤纸过滤于烧杯中，残渣再用30mL丙酮按上法再提取一次。用30mL丙酮分次洗涤残渣，洗液并入烧杯中，于水浴（50℃）上挥发浓缩近干。

3.1 Extraction
Weigh 20g of rice sample grinded and passed the 20 mesh sieve to a flask with stopper, add 50 ml of acetone, shake for 30 minutes by the electrodynamic shaker, filter to a beaker through quick qualitative filter paper, extract the residue once more using the above method by 30 ml of acetone. Wash the residue by 30 ml of acetone in several times, combine the washings to a beaker, vaporize to dry on the water bath of 50℃.

4.2.1.层析柱的制备
Column,（φ20mm×200mm）层析柱（φ20mm×200mm）下端装入2cm高的无水硫酸钠，称取10 g硅镁吸附剂装入层析柱，柱上端再装2cm高的无水硫酸钠。用20mL二氯甲烷淋洗净化柱，并弃去淋洗液。

3.2.1 Preparation of column
Insert 2 cm of anhydrous sodium sulfate in the bottom of the column ( Φ20mm x200mm), pack 10 g of silicon-magnesium adsorbent into the column, pack 2 cm of anhydrous sodium sulfate in the upside of the column. Elute by 20 ml of dichloromethane, discard the eluate.

4.2.2.样品提取液的净化
用少量二氯甲烷溶解样品提取浓缩液，倾入层析柱。用100mL二氯甲烷洗脱，洗脱速度为0.5～1.0mL／min。收集洗脱液于K.D浓缩器中，减压浓缩至1.0mL以下。用丙酮洗涤K.D浓缩器继续浓缩至1.0mL以下。最后用丙酮定容至1.0mL，待测。
3.2.2 Purification of the extract
Dissolve the concentration of the extract by little amount of dichloromethane and pour into the column. Elute using 100ml of dichloromethane with a speed of 0.5～1.0mL／min. Collect the eluate to the K.D. concentrator, concentrate by reducing the pressure until the volume is lower than 1.0 ml, wash the K.D. concentrator using acetone, continue to concentrate
volume is lower than 1.0 ml. Make up to volume of 1.0 ml using acetone.

4.3.气相色谱参考条件
3.3 Chromatographic conditions (typical)
4.3.1.色谱柱：φ3mm×110mm玻璃柱，内装涂溃2％OV－17chromosorb W AW-DMCS（60～80目）。
Column, glass column, φ3mm×110mm, coated with 2％OV－17chromosorb W AW-DMCS（60～80 mesh）
4.3.2.温度：柱温控制在235℃，检测器和汽化室温度均控制在260℃。
Temperature: Column, 235℃
Detector and vaporizer, 260℃
4.3.3.气体：氮气：（纯度≥99.998％）70mL／min；氢气：68.7kPa；空气：88.3kPa。
Gas: Nitrogen ( purity ≥99.998%) 70ml/min;
Hydrogen: 68.7 kPa;
Air: 88.3 kPa

4.测定
吸取稻瘟灵标准使用液和样品净化液各1.0μL，分别重复3次测定。以保留时间定性，以样品的平均峰高值与标准的平均峰高值比较定量。在上述色谱条件下，稻瘟灵的保留时间约为2.6min。
3.4 Determination
Pipette 1.0 μl of the standard solution and 1.0 μl of the test solution respectively, and repeat the determination for three times. Qualify by the retention time, quantify by comparing the average peak height of the test sample and the standard sample. The retention time of isoprothiolane is 2.6min under the above chromatographic conditions.

4.1 Calculation
The square of the concentration of sulfur in isoprothiolane is in the direct ration with the peak height at the wave length of 394nm when using FPD. When the injected volume of standard solution is the same as the test solution, the concentration of isoprothiolane in the test sample is calculated by the followed formula:

Ci2＝    Cs2×hi    ……………………………（1）
    hs   
where：
Ci——Concentration of isoprothiolane in the test solution, g／mL；
Cs——concentration of isoprothiolane in the standard solution,μg／mL；
hi——Peak height of isoprothiolane in the test solution, mm or mV；
hs——Peak height of isoprithiolane in the standard solution, mm或mV。
The concentration of isoprothiolane in the test sample is calculated by the followed formula:
X＝    Ci×Vi    …………………………（2）
    m   
Where：
X——Isoprothiolane content in the test sample，mg／kg；
Vi——Final volume of the test solution,mL；
m——Mass of the test sample，g。

5. Allowance
本标准检出限为0.26ng，若取20.0g大米样品，其最低检出浓度为0.013mg／kg；标准曲线的线性范围为0～15ng；平均添加回收率为108.4％；相对标准偏差≤10％。
The detect limit is 0.26mg. The lowest concentration detectable should be 0.013mg/kg if the amount of the rice sample is 2.0 g. The linear of the standard curve is0-15 mg; the average spiked recovery is 108.4%, and the relative standard deviation is not greater than 10%.