目的建立總有機(jī)碳（TOC）分析技術(shù)實(shí)現(xiàn)快速分析注射用丹參多酚酸主要原料丹參多酚酸的生產(chǎn)設(shè)備清洗殘留。方法對(duì)TOC法的專屬性、準(zhǔn)確度、精密度（重復(fù)性與中間精密度）、線性、檢測(cè)限、定量限與耐用性進(jìn)行驗(yàn)證。將不同含碳濃度的丹參多酚酸樣品溶液滴于不銹鋼板上，擦拭取樣，計(jì)算取樣回收率。結(jié)合方法學(xué)研究數(shù)據(jù)評(píng)價(jià)TOC法用于丹參多酚酸生產(chǎn)設(shè)備清洗殘留檢測(cè)的效果。結(jié)果空白溶劑與空白棉簽對(duì)測(cè)定丹參多酚酸生產(chǎn)設(shè)備清洗殘留的干擾較小；準(zhǔn)確度的平均回收率為103%，重復(fù)性與中間緊密度的RSD值均小于3%；丹參多酚酸理論含碳質(zhì)量濃度在0~30 μg/mL線性關(guān)系良好（r=0.999 9），定量限為55 ng/mL，檢測(cè)限為18 ng/mL。供試品溶液在冰箱2~10℃中儲(chǔ)存的有效期為48 h，酸堿耐用性范圍為5~9；平均取樣回收率為100%。設(shè)備改造的清潔驗(yàn)證實(shí)驗(yàn)中，丹參多酚酸生產(chǎn)設(shè)備清洗殘留的檢測(cè)結(jié)果最大值為2.22 μg/mL，均低于驗(yàn)證標(biāo)準(zhǔn)。結(jié)論 TOC分析方法快速、準(zhǔn)確、簡(jiǎn)便，可用于丹參多酚酸生產(chǎn)設(shè)備的殘留檢測(cè)，為設(shè)備清洗潔凈程度的判斷提供有力依據(jù)。

Objective To establish total organic carbon (TOC) analysis technology to realize rapid analysis of production equipment cleaning residue for salvianolic acids, the main raw material of Salvianolic Acids for Injection. Methods TOC method was verified for specificity, accuracy, precision, linearity, limit of detection, limit of quantitation and robustness. Drop the salvianolic acids sample solutions with different carbon concentrations on the stainless steel plate, wipe the samples, and calculate the sampling recovery rate. Combining methodological research data to evaluate the effect of TOC method in the detection of production equipment cleaning residue for salvianolic acids. Results Blank solvent and blank cotton swabs had little interference in the determination of salvianolic acids production equipment cleaning residue. The mean recovery in accuracy test was 103%. Both the RSDs in reproducibility and intermediate precision tests were less than 3%. Good linearity (r = 0.999 9) was observed in the standard curves of theoretical carbon content in the range of 0 — 30 μg/mL. LOD was 18 ng/mL and LOQ was 55 ng/mL. The validity period of the test solution stored in the refrigerator (2 — 10 ℃) was 48 h, and the acid-base durability range was 5 — 9. The average sampling recovery rate was 100%. In the cleaning verification experiment of equipment modification, the maximum detection result of the production equipment cleaning residue for Salvianolic Acids was 2.22 μg/mL, which are all lower than the verification standard. Conclusion Total organic carbon (TOC) analysis method is rapid, accurate and simple. It can be used for residue detection of salvianolic acids production equipment, which provides a strong basis for the determination of the cleanliness of equipment cleaning.

R927.2

天津市科技重大專項(xiàng)與工程（18ZXXYSY00120）