Method for simultaneously detecting laxative components in weight-losing product based on UPLC-MS/MS
A detection method and component technology, applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of poor reproducibility, complicated steps, insufficient matrix, etc., and achieve the effect of small recovery loss, good filtration effect, and simple steps
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Embodiment 1
[0031] refer to figure 1 As shown, the present invention discloses a method for simultaneous detection of laxative ingredients in weight loss products based on UPLC-MS / MS. The laxative ingredients include 8 ingredients, namely phenolphthalein, emodin, sodium picosulfate, bisacodyl, diacetate phenbutanol, sennoside A, sennoside B and aloin, and the simultaneous detection method includes the following steps:
[0032] S1. Preparation of standard products: Weigh the standard products of 8 kinds of laxative ingredients, weigh 10 mg, place them in 10 mL volumetric flasks, add methanol solution to dissolve and dilute to volume, and obtain a single standard stock solution.
[0033] S2. Preparation of standard solution: pipette the single standard stock solution in step S1 respectively, add methanol solution to dilute and prepare a mixed standard solution with a concentration of 100 ng / mL.
[0034] S3. Sample pretreatment: Weigh samples from weight loss products and place them in a 50...
Embodiment 2
[0055] The preparation of standard products, preparation of standard solutions, sample pretreatment, and on-machine detection and analysis steps in this embodiment are the same as those in Example 1. This embodiment adopts the external standard method for quantification, which is used to obtain the detection limit and quantification limit of the laxative components.
[0056] The linear range of the concentration of bisacodyl in the detection items of laxative ingredients is set at 0.5-10ng / mL, and the other phenolphthalein, emodin, sodium picosulfate, diacetate, sennoside A, sennoside B and aloin The linear range of the concentration of the project is set at 5-100ng / mL, and the correlation coefficient R of the curve equation within the concentration range 2 >99, with a good linear relationship; the lower limit of detection of the corresponding concentration was obtained when the signal-to-noise ratio was 3 times, and the lower limit of quantification of the corresponding concen...
Embodiment 3
[0062] In this embodiment, the configuration standard product, configuration standard solution, sample pretreatment and on-machine detection and analysis steps are the same as in Embodiment 1. The samples in this embodiment are undetected tablets, capsules or liquid weight loss products based on the pre-test results. Base, spiked at two levels of low concentration and high concentration, respectively, where the added concentrations of bisacodyl were 0.2 μg / kg and 1.0 μg / kg, and the added concentrations of other laxative ingredients were 2 μg / kg and 10 μg / kg , and do parallel tests (n=6) at the same time to obtain the recovery rate and RSD of the laxative components of different bases; the recovery rate of standard addition=(measured value of the added standard sample-measured value of the sample) / amount of added standard×100%; The recoveries and RSDs of the laxative ingredients are shown in Table 4.
[0063] The standard recovery rate and RSD of table 4 laxative composition
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