In order to establish an HPLC-MS/MS method for detecting progesterone in raw milk,raw milk was extracted with methanol,and then determined by HPLC-MS/MS after the purification with a C18 solid phase extraction column....In order to establish an HPLC-MS/MS method for detecting progesterone in raw milk,raw milk was extracted with methanol,and then determined by HPLC-MS/MS after the purification with a C18 solid phase extraction column. Qualitative determination was performed according to retention time and selective ion abundance ratio,and quantification was performed by external standard method. The results showed that progesterone had a good linear relation in the range of0. 1-5. 0 ng/ml,with a correlation coefficient of 0. 999 9. The detection limit of the established method was 0. 02 μg/kg,and the quantification limit was0. 04 μg/kg. In the standard addition range of 0. 1-5. 0 ng/ml,the recovery ranged from 79. 6% to 105. 1%,with relative standard deviation≤8. 9%. Compared with the industry standard,the detection limit and the quantification limit of the established method are significantly reduced,and the sensitivity of the method is enhanced,so this method is suitable for the detection of progesterone residue in fresh milk in pastures.展开更多
基金Supported by Science and Technology Open Cooperation Project of Henan Province(162106000017)Science and Technology People-benefiting Plan Project of Henan Province(152207110004)+1 种基金Major Science and Technology Program of Henan Province(16110051020)Puyang Science and Technology Plan Project(160215)
文摘In order to establish an HPLC-MS/MS method for detecting progesterone in raw milk,raw milk was extracted with methanol,and then determined by HPLC-MS/MS after the purification with a C18 solid phase extraction column. Qualitative determination was performed according to retention time and selective ion abundance ratio,and quantification was performed by external standard method. The results showed that progesterone had a good linear relation in the range of0. 1-5. 0 ng/ml,with a correlation coefficient of 0. 999 9. The detection limit of the established method was 0. 02 μg/kg,and the quantification limit was0. 04 μg/kg. In the standard addition range of 0. 1-5. 0 ng/ml,the recovery ranged from 79. 6% to 105. 1%,with relative standard deviation≤8. 9%. Compared with the industry standard,the detection limit and the quantification limit of the established method are significantly reduced,and the sensitivity of the method is enhanced,so this method is suitable for the detection of progesterone residue in fresh milk in pastures.
