A method of validating data produced from a multiplexing process on an analytical instrument comprising an ion mobility spectrometer and a time-of-flight mass spectrometer, the method comprising: (i) using a pseudorandom sequence to encode multiplexed time segments of data by modulating introduction of analytes to the ion mobility spectrometer based on the pseudorandom sequence, wherein the pseudorandom sequence consists of first bits each having a first value corresponding to a peak and second bits each having a second value corresponding to not a peak; (ii) generating received multiplexed intensity data with the time-of-flight mass spectrometer for the time segments; (iii) applying a Hadamard transform corresponding to the pseudorandom sequence to the received multiplexed intensity data to generate demultiplexed data for the time segments; (iv) aligning the pseudorandom sequence to the multiplexed intensity data for the time segments by aligning a first one of the first bits with a positive value of the multiplexed intensity data; (v) calculating a score by summing each positive value in the multiplexed intensity data for the time segments corresponding to a respective one of the first bits in the pseudorandom sequence; (vi) repeating (iv) and (v) for each of the positive values of the multiplexed intensity data to find the largest score and a valid demultiplexed value of the multiplexed time segments of data; and (vii) subtracting the valid multiplexed value from other multiplexed values that correspond to a one of the first bits in the pseudorandom sequence when aligned with the valid multiplexed value to create a second multiplexed segment of values; wherein said first value is 1 and wherein aligning the pseudorandom sequence to the multiplexed intensity data includes aligning a first '1' bit of the pseudorandom sequence to a positive value of the multiplexed intensity data; and wherein said summing comprises summing the multiplexed intensity data values that correspond to a '1' in the pseudorandom sequence. (i) using a pseudorandom sequence to encode multiplexed time segments of data by modulating introduction of analytes to the ion mobility spectrometer based on the pseudorandom sequence, wherein the pseudorandom sequence consists of first bits each having a first value corresponding to a peak and second bits each having a second value corresponding to not a peak; (ii) generating received multiplexed intensity data with the time-of-flight mass spectrometer for the time segments; (iii) applying a Hadamard transform corresponding to the pseudorandom sequence to the received multiplexed intensity data to generate demultiplexed data for the time segments; (iv) aligning the pseudorandom sequence to the multiplexed intensity data for the time segments by aligning a first one of the first bits with a positive value of the multiplexed intensity data; (v) calculating a score by summing each positive value in the multiplexed intensity data for the time segments corresponding to a respective one of the first bits in the pseudorandom sequence; (vi) repeating (iv) and (v) for each of the positive values of the multiplexed intensity data to find the largest score and a valid demultiplexed value of the multiplexed time segments of data; and (vii) subtracting the valid multiplexed value from other multiplexed values that correspond to a one of the first bits in the pseudorandom sequence when aligned with the valid multiplexed value to create a second multiplexed segment of values; wherein said first value is 1 and wherein aligning the pseudorandom sequence to the multiplexed intensity data includes aligning a first '1' bit of the pseudorandom sequence to a positive value of the multiplexed intensity data; and wherein said summing comprises summing the multiplexed intensity data values that correspond to a '1' in the pseudorandom sequence.