食品与药品
食品與藥品
식품여약품
FOOD AND DRUG
2015年
3期
179-182,183
,共5页
头孢地嗪钠%含量测定%有关物质%高效液相色谱法
頭孢地嗪鈉%含量測定%有關物質%高效液相色譜法
두포지진납%함량측정%유관물질%고효액상색보법
cefodizime sodium%assay%related substance%HPLC
目的：建立孢地嗪钠含量和有关物质检测方法。方法采用高效液相色谱法（HPLC），以十八烷基硅烷键合硅胶为填充剂（250 mm×4.6 mm，5μm)；流动相A为pH 3.2醋酸铵溶液（取醋酸铵1.9 g，加水2000 mL溶解，甲酸调pH 3.2），流动相B为乙腈，流速为1.0 mL/min，线性梯度洗脱；检测波长254 nm；柱温35℃。结果各杂质峰与主成分峰能完全分离，头孢地嗪钠的检测限为0.056μg/mL，定量限为0.22μg/mL，头孢地嗪钠在0.15~769.2μg/mL范围内线性关系良好（r＞0.999），80%，100%，120%浓度下各进3个平行样，测得含量的RSD为0.25%。通过酸、碱、氧化、高温、光照对头孢地嗪钠进行破坏，本法可使头孢地嗪钠及其降解产物得到较好分离，可作为稳定性指示方法用于头孢地嗪钠的稳定性检测。结论本方法符合方法学验证要求，可用于头孢地嗪钠含量和有关物质的检测。
目的：建立孢地嗪鈉含量和有關物質檢測方法。方法採用高效液相色譜法（HPLC），以十八烷基硅烷鍵閤硅膠為填充劑（250 mm×4.6 mm，5μm)；流動相A為pH 3.2醋痠銨溶液（取醋痠銨1.9 g，加水2000 mL溶解，甲痠調pH 3.2），流動相B為乙腈，流速為1.0 mL/min，線性梯度洗脫；檢測波長254 nm；柱溫35℃。結果各雜質峰與主成分峰能完全分離，頭孢地嗪鈉的檢測限為0.056μg/mL，定量限為0.22μg/mL，頭孢地嗪鈉在0.15~769.2μg/mL範圍內線性關繫良好（r＞0.999），80%，100%，120%濃度下各進3箇平行樣，測得含量的RSD為0.25%。通過痠、堿、氧化、高溫、光照對頭孢地嗪鈉進行破壞，本法可使頭孢地嗪鈉及其降解產物得到較好分離，可作為穩定性指示方法用于頭孢地嗪鈉的穩定性檢測。結論本方法符閤方法學驗證要求，可用于頭孢地嗪鈉含量和有關物質的檢測。
목적：건립포지진납함량화유관물질검측방법。방법채용고효액상색보법（HPLC），이십팔완기규완건합규효위전충제（250 mm×4.6 mm，5μm)；류동상A위pH 3.2작산안용액（취작산안1.9 g，가수2000 mL용해，갑산조pH 3.2），류동상B위을정，류속위1.0 mL/min，선성제도세탈；검측파장254 nm；주온35℃。결과각잡질봉여주성분봉능완전분리，두포지진납적검측한위0.056μg/mL，정량한위0.22μg/mL，두포지진납재0.15~769.2μg/mL범위내선성관계량호（r＞0.999），80%，100%，120%농도하각진3개평행양，측득함량적RSD위0.25%。통과산、감、양화、고온、광조대두포지진납진행파배，본법가사두포지진납급기강해산물득도교호분리，가작위은정성지시방법용우두포지진납적은정성검측。결론본방법부합방법학험증요구，가용우두포지진납함량화유관물질적검측。
Objective To establish a method for determination of cefodizime sodium and the related substances. Methods HPLC was employed with C18 (250 mm×4.6 mm, 5 μm) as column filler, the linear gradient elution was carried out with ammonium acetate buffer solution (dissolve 1.9 g of ammonium acetate in 2000 mL of water, adjust pH to 3.2) as mobile phase A and acetonitrile as mobile phase B, the flow rate was 1.0 mL/min, the detection wavelength was 254 nm and the column temperature was 35℃.Results Cefodizime sodium and its impurities could be separated completely. The LOD of cefodizime sodium was 0.056 μg/mL and LOQ was 0.22 μg/mL, the linear relationship was good within 0.15-769.2 μg/mL (r>0.999),RSD of assay at 80 %, 100 %, 120 % levels was 0.25 %. Destruction by acid, alkali, oxidation, high temperature and light was carried out, and the peaks of degradation products and cefodizime sodium could be separated well. This method was considered as stability-indicating.Conclusion The method has been validated and can be used for the determination of cefodizime sodium and the related substances.
