海螵蛸质量标准研究

Quality standard for cuttlebone

目的建立海螵蛸质量标准。方法对浙江、山东、江苏、福建、广东、广西、云南、海南和辽宁省产的30批海螵蛸进行了显微鉴别并对其碳酸钙含有量、5种重金属[铜（Cu）、砷（As）、镉（Cd）、铅（Pb）和汞（Hg）]和水分、总灰分及酸不溶性灰分进行了测定。结果碳酸钙在0.050 1-0.1601g范围内线性关系良好（r=0.999 5）;平均加样回收率为100.9%,RSD 0.24%（n=9）;精密度试验RSD 0.10%（n=5）;重复性试验RSD0.13%（n=5）;稳定性试验RSD 0.26%（n=5）。不同产地海螵蛸的碳酸钙含有量范围为83.20%-95.42%,平均值为90.09%;水分测定结果为0.92%-2.71%,平均值为1.79%;总灰分结果为83.50%-95.87%,平均值为90.66%;酸不溶性灰分结果为0.01%-0.34%,平均值为0.17%。2个样本含铜量超过限度、9个样本的含镉量超过限度。结论规定碳酸钙含有量不得少于86.0%,可使93%的样本被覆盖在合格范围内;海螵蛸水分不得高于2.5%,可使96%的样本被覆盖在合格范围内。

AIM To establish the quality standard for cuttlebone（ Sepiae endoconcha）.METHODS The identification of the microscopic characteristics and the determinations of Ca CO3,water content,ash content,acidinsoluble ash and five kinds of heavy metals of cuttlebone from Zhejiang,Shandong,Jiangsu,Fujian,Guangdong,Guangxi,Yunnan,Hainan and Liaoning Province were carried out.RESULTS The methodology validation for the assay of Ca CO3 presented the good linearity in the range of 0.050 1- 0.160 1 g,and the average recovery was100.9% with the RSD 0.24%（ n = 9）.In addition,the RSDs of reproducibility,precision and stability experiments were 0.13%,0.10% and 0.26%,respectively.As a result,the content of Ca CO3,water,ash and acid-insoluble ash of cuttlebone from different batches ranged from 83.20% to 95.42%,0.92% to 2.71%,83.50% to95.87% and 0.01% to 0.34%,respectively,and their averages were 90.09%,1.79%,90.66% and 0.17%,correspondingly.Besides,Cu content of two samples was out of limitation,the same to Cd content of nine samples.CONCLUSION If the standard of Ca CO3 content is higher than 86.0%,it covers 28 out of 30 samples.Otherwise water content is lower than 2.5%,it covers 29 out of 30 samples of cuttlebone.