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China Surfactant Detergent & Cosmetics ›› 2023, Vol. 53 ›› Issue (2): 187-192.doi: 10.3969/j.issn.1001-1803.2023.02.009
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Xue Jing,Yang Qingyun,Huang Baobin(
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Received:2022-03-31
Revised:2023-01-30
Online:2023-02-22
Published:2023-02-23
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Xue Jing, Yang Qingyun, Huang Baobin. Analysis on the “Technical Guidelines for the Development and Drafting of Supplementary Test Methods for Cosmetics”[J].China Surfactant Detergent & Cosmetics, 2023, 53(2): 187-192.
Tab. 1
Comparison of the method validation items and indicators of the supplementary testing methods for cosmetics and drugs"
| 考察项目 | 化妆品补充检验方法 | 药品补充检验方法 |
|---|---|---|
| 特异性/专属性 | 分析空白基质和添加了标准物质的空白基质，考察空白基质中的化合物是否干扰测定 | 定性检查：阴性或空白样品，结构相似或组分中的有关化合物，应呈阴性反应 限量检查/含量测定：采用色谱法和其他分离方法应附代表性图谱，色谱法中分离度应符合要求 |
| 准确度 | 在规定的线性范围内，设计高中低3个浓度水平的添加试验，每个水平重复至少6次，计算平均回收率。参考范围见 在方法定量限、2倍定量限、10倍定量限三个浓度水平进行回收率试验；对于有限量值的，在0.5倍、1倍、2倍限量值三个浓度水平进行回收率试验，当限量值为定量限时，在2倍和10倍限量值两个浓度水平进行回收率试验；对于暂无限量值的，在方法定量限和两个常见浓度水平进行回收率试验 | 在规定的线性范围内，取100%浓度水平的供试品，至少测定6份，计算平均回收率；或设计至少3种不同浓度水平，每种浓度至少测定3份供试品，计算平均回收率。参考范围见 |
| 精密度 （重复性、重现性） | 典型基质均应考察精密度，至少进行高中低3个浓度水平的试验，添加水平的要求同准确度试验，每个水平重复至少6次，计算相对标准偏差（RSD）。参考范围见 | 取100%浓度水平的供试品，至少测定6份，计算相对标准偏差（RSD）；或设计至少3种不同浓度水平，每种浓度至少测定3份供试品，计算RSD。参考范围见 |
| 检测限和 定量限 | 检测限和定量限应该满足检测方法的预期用途。在定量限浓度水平下得到的回收率和精密度应满足上述 | 检测限：通常采用信噪比（S/N）法，以S/N为3∶1时的供试品浓度为检测限。应附测定图谱 定量限：通常采用信噪比（S/N）法，以S/N为10∶1时的供试品浓度为定量限。应附测定图谱，测定结果应符合上述准确度（ |
| 线性和线性 范围 | 至少进行5个浓度水平，应列出标准曲线方程、相关系数，必要时给出典型色谱图。应比较不加基质的标准曲线和加基质的标准曲线的差异。线性范围应尽可能覆盖一个以上数量级 | 应在设计的浓度范围内测定线性关系，至少制备5个浓度水平，应列出回归方程、相关系数、残差平方和、线性图。线性范围应根据方法的具体应用和线性、准确度、精密度结果及要求确定。含量测定的线性范围一般为测定浓度的80%~120% |
| 耐用性 | 方法研制时应考虑其耐用性，测定条件小的变动应能满足系统适用性试验要求。如测试条件苛刻，应在方法中注明可以接受变动的范围 | |
Tab. 2
Recovery reference range of the supplementary testing methods for cosmetics"
| 检测目标物含量/（mg/kg） | 回收率限度/% |
|---|---|
| >100 | 95~105 |
| 1~100 | 90~110 |
| 0.1~1 | 80~110 |
| ≤0.1 | 60~120 |
Tab. 3
Recovery reference range of the supplementary testing methods for drugs"
| 检测目标物含量 | 回收率限度/% | ||
|---|---|---|---|
| % | ppm或ppb | g/g | |
| 1 | 10 000 ppm | 0.01 | 92~105 |
| 0.1 | 1 000 ppm | 0.001 | 90~108 |
| 0.01 | 100 ppm | 0.000 1 | 85~110 |
| 0.001 | 10 ppm | 0.000 01 | 80~115 |
| 0.000 1 | 1 ppm | 0.000 001 | 75~120 |
| 0.000 001 | 10 ppb | 0.000 000 01 | 70~125 |
Tab. 4
Precision reference range of the supplementary testing methods for cosmetics"
| 检测目标物含量/ （mg/kg） | 重复性 （RSDr）/% | 重现性 （RSDR）/% |
|---|---|---|
| 100~1 000 | ≤ 3.8 | ≤19 |
| 10~100 | ≤ 5.3 | ≤19 |
| 1~10 | ≤ 7.5 | ≤19 |
| 0.1~1 | ≤11 | ≤25 |
| 0.01~0.1 | ≤15 | ≤34 |
| 0.001~0.01 | ≤21 | ≤46 |
| 0.000 1~0.001 | ≤30 | ≤54 |
| ≤0.000 1 | ≤43 | ≤54 |
Tab. 5
Precision reference range of the supplementary testing methods for drugs"
| 检测目标物含量 | 重复性（RSDr）/% | 重现性（RSDR）/% | ||
|---|---|---|---|---|
| % | ppm或ppb | g/g | ||
| 1 | 10 000 ppm | 0.01 | ≤ 2 | ≤ 4 |
| 0.1 | 1 000 ppm | 0.001 | ≤ 3 | ≤ 6 |
| 0.01 | 100 ppm | 0.000 1 | ≤ 4 | ≤ 8 |
| 0.001 | 10 ppm | 0.000 01 | ≤ 6 | ≤11 |
| 0.000 1 | 1 ppm | 0.000 001 | ≤ 8 | ≤16 |
| 0.000 001 | 10 ppb | 0.000 000 01 | ≤15 | ≤32 |
| [1] | Guo Ting. Fully open a new chapter in cosmetics supervision and management-Analysis of the four highlights of “Regulations on Supervision and Administration of Cosmetics”[N]. Zhongguo Yiyao Bao, 2020-06-30 (1). |
| [2] | National Medical Products Administration. Announcement on the issuance of “Management Procedures of Supplementary Testing Methods for Cosmetics” and “Development and Drafting Technical Guide of Supplementary Testing Methods for Cosmetics”(No.28, 2021)[EB/OL].(2021-04-28) [2022-03-16]. https://www.nmpa.gov.cn/zhuanti/hzhpxch2021/hzhp2021fgwj/20210428140400103.html |
| [3] | National Medical Products Administration. Announcement on the issuance of “Development Guide of Supplementary Testing Methods for Drugs”(No.7, 2018)[EB/OL]. (2018-01-09) [2022-03-16]. https://www.nmpa.gov.cn/yaopin/ypggtg/ypqtgg/20180109162601653.html |
| [4] | Li Mingyang. Cosmetic chemistry[M]. Beijing: Science Press, 2002. |
| [5] | Zhang Yanshu, Lin Zhenhua, Hu Yuling, et al. Advance on pretreatment methods for cosmetic samples analysis[J]. Journal of Instrumental Analysis, 2016, 35 (2):127-136. |
| [6] | Chinese Pharmacopoeia Commission. Pharmacopoeia of the People’ s Republic of China 2020 Volume Ⅳ [S]. Beijing: China Medical Science Press, 2020: 480-483. |
| [7] | Cao Jin, Zhang Qingsheng. Current status and development of chemical analysis on cosmetic in China[J]. Chinese Pharmaceutical Affairs, 2011, 25 (4):79-81. |
| [8] | Cosmetics Standards Expert Committee of National Medical Products Administration. Safety and technical standards for cosmetics (2015 edition)[M]. Beijing: People’s Medical Publishing House, 2017. |
| [9] | Gao Jiamin, Cao Jin, Ding Hong. The comparison of cosmetic standard system and drug standard system and analysis of testing characteristics[J]. Chinese Pharmaceutical Affairs, 2017, 31 (8):887-893. |
| [10] | Wang Hongyu. Study on quality control technology of traditional chinese medicine and its cut crude drug in supplementary testing methods[J]. Journal of Clinical Medical, 2018, 5 (23):181-182. |
| [11] | Wei Feng, Cheng Xianlong, Ma lingyun, et al. Discussion on technical requirements of substitution method of reference substance used for drug standards[J]. Drug Standards of China, 2012, 13 (1):12-15. |
| [12] | Tang Hui, Ge Wenchao, Zhang Ping, et al. Detection of five illegally added chemical medicine components in sedative-hypnotic drugs in traditional chinese medicines and health foods using digital reference substances[J]. Anhui Medical and Pharmaceutical Journal, 2012, 16 (11):1601-1603. |
| [13] | Zhang Ping, Wu Min, Tang Hui, et al. Rapid determination of eight tetracycline residues in eggs by a search platform using numerical reference substance database based on HPLC-DAD spectrums[J]. Anhui Medical and Pharmaceutical Journal, 2015, 19 (2):252-256. |
| [14] | National Medical Products Administration. Announcement on the update of catalogue of prohibited raw materials for cosmetics (No.74, 2021)[EB/OL].(2021-05-28) [2022-03-16]. https://www.nmpa.gov.cn/xxgk/ggtg/qtggtg/20210528174051160.html?type=pc&m= |
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