HPLC法同时测定苍山蒜米中双乙酸钠和丙酸钙含量

Determination of sodium diacetate and calcium propionate in garlic clove by HPLC

以山东苍山蒜米为实验材料,建立了同时测定蒜米中双乙酸钠和丙酸钙含量的高效液相色谱法（HPLC）。蒜米中双乙酸钠经磷酸酸化后转化成乙酸,丙酸钙经酸化后变为游离丙酸,二者预处理后经超声波水浴提取20 min,加磷酸调节收集液p H至3,经高效液相色谱测定。方法采用单泵色谱柱Arcus EP-C18（5μm,150 mm×4.6 mm）,柱温：20℃;流动相：1.5g/L磷酸二氢钾溶液（调节p H=3.0）;流速1.0 m L/min,紫外检测波长214 nm,进样量10μL。结果表明：双乙酸钠、丙酸钙浓度在0.20-2.00 mg/m L范围内线性关系良好,相关系数分别为0.99987和0.99935,均大于0.999;出峰时间分别为2.60、6.90 min;当信噪比S/N=3、次数n=6时,双乙酸钠、丙酸钙最低检出量为1.70 mg/kg,平均回收率是91.32%和89.79%,相对标准偏差是1.78%和1.64%,均小于5%。该方法快速简便,准确灵敏,回收率高,可用于同时测定蒜米中双乙酸钠和丙酸钙含量。

Shandong Cangshan garlic clove was used as test material,and a new HPLC method for determing sodium diacetate and calcium propionate contents in garlic was established.Sodium diacetate could convert to acetic acid after acidification by phosphoric acid and calcium propionate was transformed to free propionic acid using acidification in garlic.After acidification,both acid was extracted by ultrasonic water bath for 20 min,and then the p H of regulating collecting liquid was adjusted around 3 using phosphate acid,finally were tested by high performance liquid chromatography（HPLC）.This extracts were separated on a Arcus EP-C18 analytical column（5 μm,4.6 mm×150 mm）;the column temperature：25 ℃;the mobile phase：1.5 g/L potassium dihydrogen phosphate solution（p H=3.0）;the flow rate：1.0 m L/min;UV detection wavelength：214 nm;injection volume：10 μL.The results showed that：the calibration curves of sodium diacetate and calcium propionate performed good linear relationship when the concentration ranged from 0.20-2.00 mg/m L（r=0.99987 and 0.99935,respectively）,and the correlation coefficient were higher than 0.999;the peak time of sodium diacetate and calcium propionate showed at 2.60 min and 6.90 min,respectively.As SNR S/N=3,frequency n=6,the minimum detectable amount of sodium diacetate and calcium propionate were 1.70 mg/kg,and the average recovery were 91.32% and 89.79%,respectively;the relative standard deviation were 1.78% and 1.64%,respectively,（〈5%）.Therefore,this method has some advantages,such as quick,easy,accurate,sensitive and high recovery and can be used to determine simultaneously the content of sodium diacetate and calcium propionate in garlic clove.